CN101603210A - String is made the production method of viscose - Google Patents
String is made the production method of viscose Download PDFInfo
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Abstract
The invention discloses string and make the production method of viscose, its step is as follows: alkali steeping obtains slurry congee; Slurry congee falls poly-in high temperature aerobic container; Fall the squeezing of poly-back and obtain the alkali fibre; With the fine viscose that generates of alkali.The present invention directly forces degradation technique to make the method for viscose with plant fiber material such as papermaking level pulpboard by wet, this method not only greatly reduces production cost, reduced pollution, and can fully grasp the raw-material buying initiative of pulp, greatly alleviated the raw-material buying pressure of pulp.And the two-part that overcomes the existence of employing pulp modified production process production viscose is produced the drawback that viscose brings.
Description
Technical field
The present invention relates to the method that the wet method mandatory down is separated the manufactured cellulose fibre in the chemical fibre manufacturing, particularly a kind of method of utilizing string (as the papermaking level pulpboard) directly to make viscose filament yarn/weak point silk.
Background technology
The main form of plant fiber material has slurry to pull shape, bulk, Powdered, graininess, wherein papermaking level pulpboard (the string pulpboard that the degree of polymerization is high) has very large output in the whole world, China's annual import papermaking level pulpboard is more than 8,000,000 tons, self-produced papermaking level pulpboard is more than 3,000,000 tons, so the pulpboard resource of papermaking level is quite abundant, and this pulpboard price very low (with respect to viscose filament yarn/weak point silk pulp).If these plant fiber materials can apply to viscose filament yarn/weak point silk and produce, not only can reduce production costs greatly, can also alleviate a raw material difficult problem in short supply.But because the degree of polymerization of this papermaking level pulpboard is very high, usually all more than 1000, and the content of chemical cellulose is low, can only be used for paper industry, can not directly be used for carrying out viscose filament yarn/weak point silk and produce.Therefore must carry out a series of degenerative treatments to the papermaking level pulpboard, cellulosic average degree of polymerization is significantly reduced, chemical cellulose content increases substantially, the fibrin reaction performance is improved significantly to satisfy the production requirement of viscose filament yarn/weak point silk.
200610021387.4 disclose a kind of Wood pomace modified producing technology, adopting the papermaking level wood-pulp board is raw materials for production, pass through paging, alkali steeping, discongest dispersion, boiling, washing, removal of impurities, bleaching, secondary washing, copy the dregs of rice, produce the dissolving grade wood pulps that can be used to produce viscose at last.Obtain just can be directly used in viscose production after the dissolving grade wood pulps.The essence of the disclosed technical scheme of this application for a patent for invention is to be used for the papermaking level pulpboard that viscose is produced, and is the dissolving grade pulp by serial operation sex change.Raw material is through obtaining viscose through conventional cellulose viscose manufacturing technique again after the sex change.Conventional cellulose viscose manufacturing technique comprises dipping, squeezing, experienced, yellow, filtration, deaeration, spinning, concise, oven dry.
200610021387.4 though patent has effectively utilized the cheap advantage of papermaking level pulpboard to produce the dissolving grade pulp of viscose production usefulness, but make viscose produce the production of one-part form production becoming two-part, produce dissolving pulp regeneration earlier and produce viscose.200610021387.4 technology still belongs to the pulp production technology, slurry after the sex change need wash according to the pulp production requirement, removal of impurities, bleaching, secondary washing, copy the dregs of rice and become the dissolving grade pulp, complex procedures, loaded down with trivial details, and can not directly be connected with cellulose viscose manufacturing technique.Make whole cellulose viscose manufacturing technique process become huge, consuming time, power consumption, equipment many, take the big and inconvenient production management of plant area.
Summary of the invention
The purpose of this invention is to provide a kind of method of directly making viscose (long filament/weak point silk) by wet pressure degradation technique with plant fiber material (as the papermaking level pulpboard), this method not only greatly reduces production cost, reduced pollution, and can fully grasp the raw-material buying initiative of pulp, greatly alleviated the raw-material buying pressure of pulp.And the two-part that overcomes the existence of 200610021387.4 patents is produced the drawback that viscose brings.
For achieving the above object, the technical solution used in the present invention is as follows:
String is made the production method of viscose, it is characterized in that step is as follows:
A, alkali steeping obtain slurry congee;
B, slurry congee fall poly-in high temperature aerobic container;
C, fall the squeezing of poly-back and obtain the alkali fibre;
D, the fine viscose that generates of usefulness alkali.
Described A operation is finished in treating tank, 60 ℃～90 ℃ of alkali liquid temperatures, concentration of lye 40g/l～100g/l, slurry congee concentration 2.0%～4.0%, preimpregnation time: 20min～40min.
60 ℃～90 ℃ of the reaction temperatures of described B operation, reaction time 200min～300min, slurry congee concentration 2.0%～4.0%, compressed air pressure 0.3Mpa～0.5Mpa.
The container of described B operation is a reactor, makes gas-solid-liquid mixing of materials even, and slurry congee descends at high-temperature oxydation and gathers reaction; Steam adds the slurry congee circulation trunk line of reactor, the circulation trunk line is divided into a plurality of arms and stretches in the reactor, an aerator is arranged on each arm of reactor outside, and compressed air adds from the aerator position, and the slurry congee behind the sufficient reacting is delivered to squeezer from the slurry congee outlet of bottom.
Described C operation adopts squeezer that slurry congee is squeezed, 60 ℃～80 ℃ of pressing temperatures, squeeze pressure 300mbar～1000mbar, the fine content 27%～40% of the fine first of the alkali after the squeezing, the fine alkali content of alkali: fine viscosity: the 9mp.s～13mpa.s of alkali 4%～7%.
The viscose production process of described D operation comprises dipping, squeezing, experienced, yellow, obtains viscose glue, and viscose glue obtains viscose, final purification through filtration, deaeration, spinning.
The slurry congee that poly-(the reduction degree of polymerization) falls in described B operation is transported to the assistant soakage bucket and stores, for squeezing is prepared.
Beneficial effect of the present invention shows:
One, the price of papermaking level pulpboard only is about 1/2nd of a fibre-grade pulp price in the market, therefore viscose filament yarn/weak point silk of making of the present invention be that viscose filament yarn/weak point of making of raw material thread is compared with the fibre-grade pulp, production cost can reduce significantly.
Two, the invention solves the problem that low first fibre, high viscosity, reactivity worth difference and the many papermaking level pulpboards of impurity directly apply to the production of viscose filament yarn/weak point silk.
Three, the present invention has greatly enriched raw-material selection autonomy, has alleviated a raw material difficult problem in short supply widely.
Four, compare with 200610021387.4 patents, need not with the papermaking level pulpboard through washing, removal of impurities, bleaching, secondary washing, copy the dregs of rice and become the dissolving grade pulp, sex change obtains directly to enter the viscose glue production link behind the alkali fibre, reduces and drops into, improved production efficiency.
Description of drawings
Fig. 1 is a flow sheet of the present invention
The specific embodiment
This patent discloses the production technology that the sex change of papermaking level pulpboard is directly produced viscose, mainly comprise alkali pre-preg, the reactor reaction, assistant soakage, operations such as squeezing, this technology has increased the reactor reaction with direct technology with dissolving grade pulp production viscose, single-steeping and single pressing 3 procedures, but omitted (200610021387.4) washing in the production of sex change pulp, removal of impurities, bleaching, secondary washing, copy operations such as the dregs of rice, be directly used in viscose production, greatly reduce raw-material price, with traditional viscose process process synthesis relatively after, can reduce production costs greatly, produce huge economic benefit.
Concrete processing step is as follows:
One, average degree of polymerization directly being dropped into treating tank greater than 1000 plant fiber material (as the papermaking level pulpboard) carries out carrying out alkali pre-preg with alkali.
Effect: make fibrous raw material become solid and mixtures of liquids, be called slurry congee on the technology, reaction simultaneously generates alkali cellulose.
Control parameter: alkali liquid temperature: 60 ℃～90 ℃ concentration of lye: 40g/l～100g/l
Slurry congee concentration: 2.0%～4.0% preimpregnation time: 20min～40min
Two, the slurry congee after the alkali pre-preg is transported to reactor, adds steam simultaneously and compressed air reacts.Steam joins on the reactor internal recycle pipeline, and compressed air is divided into four and joins respectively in reactor four aerators all around.Thereby have at high temperature under the situation of oxygen, the destruction to the cellulose cell membrane has been accelerated in catalysis, thereby reaches the quick reduction degree of polymerization, fast the purpose of stripping half fibre.
Effect: reduce the degree of polymerization of fiber, improve chemical cellulose content simultaneously.
Control parameter: reaction temperature: 60 ℃～90 ℃ reaction time: 200min～300min
Slurry congee concentration: 2.0%～4.0%
Compressed air pressure: 0.3Mpa～0.5Mpa
The reactor design: steam adds the slurry congee circulation trunk line of reactor, the trunk line that circulates then is divided into 4 arms and stretches in the reactor, an aerator is arranged on each arm of reactor outside, compressed air adds from the aerator position, a steam vent is arranged on the reactor, an overflow pipe is arranged at top, and the bottom is the outlet of slurry congee.This reactor advantage is to make gas-solid-liquid mixing of materials even, and poly-sufficient reacting falls in high-temperature oxydation.
Three, will react slurry congee that the back degree of polymerization is reduced to requirement and be transported to the assistant soakage bucket and store, for squeezing is prepared.
Effect: store slurry congee, be convenient to production control, can strengthen the stability of production simultaneously.
Four, reacted slurry congee is squeezed with squeezer, make satisfactory alkali fibre.
Effect: squeeze out unnecessary moisture content.
Control parameter: pressing temperature: 60 ℃～80 ℃ squeeze pressure: 300mbar～1000mbar
The fine content of the fine first of alkali: 27%～40%
The fine alkali content of alkali: 4%～7%
Fine viscosity: the 9mp.s～13mpa.s of alkali
Five, satisfactory alkali fibre is gone into the viscose production system.Viscose comprises short silk and long filament, and the generation operation of viscose can adopt common process, as dipping, squeezing, experienced, yellow, obtains viscose glue, and viscose glue obtains viscose, final purification through filtration, deaeration, spinning.
The main form of the alleged plant fiber material of this patent has slurry to pull shape, bulk, Powdered, graininess, and wherein the papermaking level pulpboard is comparatively common, abundant raw material.
To help to understand the present invention by following examples, but be not limited to content of the present invention.
Embodiment 1
With average degree of polymerization is that 1200 commercially available papermaking level wood pulps is put into and feeds on the dregs of rice machine, set certain rate of feeding (10kg/min), at the alkali lye that adds 85 ℃ of concentration 85g/l, temperature, flux of alkaline liquor is 10m3/h～20m3/h, by the effect of stirring, pulp smashed with alkali lye mix fully, be mixed with concentration and be 3.0% solid-state and liquid mixture, be called slurry congee on the technology.
By delivery pump slurry congee is transported in the reactor, transporting velocity be 15m3 slurry congee/hour, utilize circulating pump in reactor, to play outer circulation simultaneously, circulation rate is 100m3/h, steam adds from the circulation trunk line, logical automatic regulating valve door is controlled the steam addition, thereby guarantee that reaction temperature is controlled at 85 ± 2 ℃, the aerator position of compressed air around above reactor adds, thereby gaseous state, liquid state and solid-state three-phase material in the reactor are fully mixed, and poly-effect falls in the oxidation that reaches a high temperature.After above-mentioned reaction, the slurry congee that fiber viscosity reaches 12 ± 3mpa.s is transported to auxiliary barrel by delivery pump, and carrying out temporary transient storage also is to get ready for next step operation squeezing.
Delivery pump by the auxiliary barrel outlet is transported to squeezer to slurry congee again, transporting velocity be 15m3 slurry congee/hour, squeezer stock tank pressure 600 ± 30mbar, the material that squeezes out is divided into two parts, a part is the alkali lye that is being mingled with small amount of fibers, another part is solid and the mixtures of liquids that has extruded excessive moisture, is called the alkali fibre on the technology.The composition control of alkali fibre requires: chemical cellulose content is 40 ± 2%, and alkalinity is 4.0 ± 0.2%.Make the fiber that meets the production requirement of viscose filament yarn/weak point after by the pulverizer of squeezer outlet the alkali fibre being pulverized.This fiber enters the production that can directly carry out viscose filament yarn/weak point thread after the former viscose filament yarn/weak point silk production system.
Embodiment 2
With average degree of polymerization is that 1000 the commercially available papermaking level cotton pulp dregs of rice are put into and feed on the dregs of rice machine, set certain rate of feeding (10kg/min), at the alkali lye that adds 80 ℃ of concentration 80g/l, temperature, flux of alkaline liquor is 10m3/h～20m3/h, by the effect of stirring, pulp smashed with alkali lye mix fully, be mixed with concentration and be 3.5% solid-state and liquid mixture, be called slurry congee on the technology.
By delivery pump slurry congee is transported in the reactor, transporting velocity be 14m3 slurry congee/hour, utilize circulating pump in reactor, to play outer circulation simultaneously, circulation rate is 100m3/h, steam adds from the circulation trunk line, logical automatic regulating valve door is controlled the steam addition, thereby guarantee that reaction temperature is controlled at 85 ± 2 ℃, the aerator position of compressed air around above reactor adds, thereby gaseous state, liquid state and solid-state three-phase material in the reactor are fully mixed, and poly-effect falls in the oxidation that reaches a high temperature.After above-mentioned reaction, the slurry congee that fiber viscosity reaches 11 ± 3mpa.s is transported to auxiliary barrel by delivery pump, and carrying out temporary transient storage also is to get ready for next step operation squeezing.
Delivery pump by the auxiliary barrel outlet is transported to squeezer to slurry congee again, transporting velocity be 14m3 slurry congee/hour, squeezer stock tank pressure 450 ± 30mbar, the material that squeezes out is divided into two parts, a part is the alkali lye that is being mingled with small amount of fibers, another part is solid and the mixtures of liquids that has extruded excessive moisture, is called the alkali fibre on the technology.The composition control of alkali fibre requires: chemical cellulose content is 40 ± 2%, and alkalinity is 3.9 ± 0.2%.Make the fiber that meets the production requirement of viscose filament yarn/weak point after by the pulverizer of squeezer outlet the alkali fibre being pulverized.This fiber enters the production that can directly carry out viscose filament yarn/weak point thread after the former viscose filament yarn/weak point silk production system.
Embodiment 3
With average degree of polymerization is that 1000 commercially available papermaking level Populus deltoides mixing pulp is put into and feeds on the dregs of rice machine, mixed proportion is 1～99, set certain rate of feeding (10kg/min), at the alkali lye that adds 80 ℃ of concentration 80g/l, temperature, flux of alkaline liquor is 8m3/h～18m3/h, by the effect of stirring, pulp is smashed with alkali lye mix fully, be mixed with concentration and be 3.5% solid-state and liquid mixture, be called slurry congee on the technology.
By delivery pump slurry congee is transported in the reactor, transporting velocity be 14m3 slurry congee/hour, utilize circulating pump in reactor, to play outer circulation simultaneously, circulation rate is 100m3/h, steam adds from the circulation trunk line, logical automatic regulating valve door is controlled the steam addition, thereby guarantee that reaction temperature is controlled at 80 ± 2 ℃, the aerator position of compressed air around above reactor adds, thereby gaseous state, liquid state and solid-state three-phase material in the reactor are fully mixed, and poly-effect falls in the oxidation that reaches a high temperature.After above-mentioned reaction, the slurry congee that fiber viscosity reaches 11 ± 3mpa.s is transported to auxiliary barrel by delivery pump, and carrying out temporary transient storage also is to get ready for next step operation squeezing.
Delivery pump by the auxiliary barrel outlet is transported to squeezer to slurry congee again, transporting velocity be 14m3 slurry congee/hour, squeezer stock tank pressure 500 ± 30mbar, the material that squeezes out is divided into two parts, a part is the alkali lye that is being mingled with small amount of fibers, another part is solid and the mixtures of liquids that has extruded excessive moisture, is called the alkali fibre on the technology.The composition control of alkali fibre requires: chemical cellulose content is 40 ± 2%, and alkalinity is 3.9 ± 0.2%.Make the fiber that meets the production requirement of viscose filament yarn/weak point after by the pulverizer of squeezer outlet the alkali fibre being pulverized.This fiber enters the production that can directly carry out viscose filament yarn/weak point thread after the former viscose filament yarn/weak point silk production system.
Embodiment 4
With average degree of polymerization is that 1100 the cotton bamboo of commercially available papermaking level mixes pulp and is put into and feeds on the dregs of rice machine, mixed proportion is 1～99, set certain rate of feeding (10kg/min), at the alkali lye that adds 85 ℃ of concentration 85g/l, temperature, flux of alkaline liquor is 10m3/h～20m3/h, by the effect of stirring, pulp is smashed with alkali lye mix fully, be mixed with concentration and be 3.0% solid-state and liquid mixture, be called slurry congee on the technology.
By delivery pump slurry congee is transported in the reactor, transporting velocity be 15m3 slurry congee/hour, utilize circulating pump in reactor, to play outer circulation simultaneously, circulation rate is 100m3/h, steam adds from the circulation trunk line, logical automatic regulating valve door is controlled the steam addition, thereby guarantee that reaction temperature is controlled at 85 ± 2 ℃, the aerator position of compressed air around above reactor adds, thereby gaseous state, liquid state and solid-state three-phase material in the reactor are fully mixed, and poly-effect falls in the oxidation that reaches a high temperature.After above-mentioned reaction, the slurry congee that fiber viscosity reaches 11 ± 3mpa.s is transported to auxiliary barrel by delivery pump, and carrying out temporary transient storage also is to get ready for next step operation squeezing.
Delivery pump by the auxiliary barrel outlet is transported to squeezer to slurry congee again, transporting velocity be 15m3 slurry congee/hour, squeezer stock tank pressure 600 ± 30mbar, the material that squeezes out is divided into two parts, a part is the alkali lye that is being mingled with small amount of fibers, another part is solid and the mixtures of liquids that has extruded excessive moisture, is called the alkali fibre on the technology.The composition control of alkali fibre requires: chemical cellulose content is 40 ± 2%, and alkalinity is 4.0 ± 0.2%.Make the fiber that meets the production requirement of viscose filament yarn/weak point after by the pulverizer of squeezer outlet the alkali fibre being pulverized.This fiber enters the production that can directly carry out viscose filament yarn/weak point thread after the former viscose filament yarn/weak point silk production system.
Embodiment 5
With average degree of polymerization is that 1200 commercially available papermaking level wood bamboo mixes pulp and is put into and feeds on the dregs of rice machine, mixed proportion is 1～99, set certain rate of feeding (10kg/min), at the alkali lye that adds 90 ℃ of concentration 90g/l, temperature, flux of alkaline liquor is 12m3/h～24m3/h, by the effect of stirring, pulp is smashed with alkali lye mix fully, be mixed with concentration and be 2.5% solid-state and liquid mixture, be called slurry congee on the technology.
By delivery pump slurry congee is transported in the reactor, transporting velocity be 18m3 slurry congee/hour, utilize circulating pump in reactor, to play outer circulation simultaneously, circulation rate is 100m3/h, steam adds from the circulation trunk line, logical automatic regulating valve door is controlled the steam addition, thereby guarantee that reaction temperature is controlled at 85 ± 2 ℃, the aerator position of compressed air around above reactor adds, thereby gaseous state, liquid state and solid-state three-phase material in the reactor are fully mixed, and poly-effect falls in the oxidation that reaches a high temperature.After above-mentioned reaction, the slurry congee that fiber viscosity reaches 12 ± 3mpa.s is transported to auxiliary barrel by delivery pump, and carrying out temporary transient storage also is to get ready for next step operation squeezing.
Delivery pump by the auxiliary barrel outlet is transported to squeezer to slurry congee again, transporting velocity be 18m3 slurry congee/hour, squeezer stock tank pressure 700 ± 30mbar, the material that squeezes out is divided into two parts, a part is the alkali lye that is being mingled with small amount of fibers, another part is solid and the mixtures of liquids that has extruded excessive moisture, is called the alkali fibre on the technology.The composition control of alkali fibre requires: chemical cellulose content is 40 ± 2%, and alkalinity is 4.2 ± 0.2%.Make the fiber that meets the production requirement of viscose filament yarn/weak point after by the pulverizer of squeezer outlet the alkali fibre being pulverized.This fiber enters the production that can directly carry out viscose filament yarn/weak point thread after the former viscose filament yarn/weak point silk production system.
Claims (7)
1, string is made the production method of viscose, it is characterized in that step is as follows:
A, alkali steeping obtain slurry congee;
B, slurry congee fall poly-in high temperature aerobic container;
C, fall the squeezing of poly-back and obtain the alkali fibre;
D, the fine viscose that generates of usefulness alkali.
2, string according to claim 1 is made the production method of viscose, it is characterized in that: described A operation is finished in treating tank, 60 ℃～90 ℃ of alkali liquid temperatures, concentration of lye 40g/l～100g/l, slurry congee concentration 2.0%～4.0%, preimpregnation time: 20min～40min.
3, string according to claim 1 is made the production method of viscose, it is characterized in that: 60 ℃～90 ℃ of the reaction temperatures of described B operation, reaction time 200min～300min, slurry congee concentration 2.0%～4.0%, compressed air pressure 0.3Mpa～0.5Mpa.
4, according to the production method of claim 1 or 3 described strings manufacturing viscoses, it is characterized in that: the container of described B operation is a reactor, makes gas-solid-liquid mixing of materials even, and slurry congee descends at high-temperature oxydation and gathers reaction; Steam adds the slurry congee circulation trunk line of reactor, the circulation trunk line is divided into a plurality of arms and stretches in the reactor, an aerator is arranged on each arm of reactor outside, and compressed air adds from the aerator position, and the slurry congee behind the sufficient reacting is delivered to squeezer from the slurry congee outlet of bottom.
5, string according to claim 1 is made the production method of viscose, it is characterized in that: described C operation adopts squeezer that slurry congee is squeezed, 60 ℃～80 ℃ of pressing temperatures, squeeze pressure 300mbar～1000mbar, the fine content 27%～40% of the fine first of the alkali after the squeezing, the fine alkali content of alkali: fine viscosity: the 9mp.s～13mpa.s of alkali 4%～7%.
6, string according to claim 1 is made the production method of viscose, it is characterized in that: the viscose production process of described D operation comprises dipping, squeezing, experienced, yellow, obtain viscose glue, viscose glue obtains viscose, final purification through filtration, deaeration, spinning.
7, string according to claim 4 is made the production method of viscose, it is characterized in that: described B operation is fallen poly-slurry congee and is transported to the assistant soakage bucket and stores, for squeezing is prepared.
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