CN107022076A - A kind of preparation method of the deep dye section of polyamide fibre 6 - Google Patents
A kind of preparation method of the deep dye section of polyamide fibre 6 Download PDFInfo
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- CN107022076A CN107022076A CN201710245038.9A CN201710245038A CN107022076A CN 107022076 A CN107022076 A CN 107022076A CN 201710245038 A CN201710245038 A CN 201710245038A CN 107022076 A CN107022076 A CN 107022076A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/092—Polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyamides (AREA)
- Artificial Filaments (AREA)
Abstract
The present invention provides a kind of preparation method of the deep dye section of polyamide fibre 6, prepares caprolactam melt liquid and deep dye additive, and according to the demand to be prepared section species, allocates the titanium dioxide seasoning liquid of respective quality concentration, standby；Then the caprolactam melt liquid prepared, deep dye additive are uniformly mixed with titanium dioxide seasoning liquid through dynamic mixer, carries out prepolymerization, final polymerization reaction, underwater cutpellet, extraction, i.e. dry cooling successively afterwards.There is higher heat resistance via section made from preparation method of the present invention, deep dye can be applied to, so as to avoid because that can not contaminate and the oxidation easily occurred and the phenomenon of yellow deeply so that product has higher added value, ultimately forms higher economic benefit.
Description
【Technical field】
The present invention relates to the preparation method of field of textiles, and in particular to a kind of preparation method of the deep dye section of polyamide fibre 6.
【Background technology】
Polyamide fibre is the synthetic fibers of the earliest industrialized production of China, with intensity height, elastic good, soft, easy dyeing
Good characteristic is waited with wear-resisting, and is widely used in garment material, knits the fields such as socks, carpet, industrial yarns.And slices of caprone is
Because of sheet granulation product obtained by the low use pellet cutting method of its melt strength in polyamide fibre production.
At present, in fierce market competition, the functional product Development and Production of differential high added value turns into polyamide fibre 6
The developing direction of industry, the new product of invention of only constantly bringing forth new ideas is that downstream textile mills create new fiber, weaves new face
Material, could win in market competition.The amido value of existing chinlon 6 section is mostly 46~48mmol/kg so that heat resistance
It is relatively low, it is impossible to carry out deep dye, the phenomenon of oxidation and yellow easily occur, so that cause added value of product relatively low, nothing
The higher economic benefit of method formation.
【The content of the invention】
The technical problems to be solved by the invention are the preparation method for providing a kind of deep dye section of polyamide fibre 6, can be made
With higher heat resistance, suitable for the section of deep dye so that product has higher added value.
The present invention is to solve above-mentioned technical problem by the following technical programs：A kind of preparation side of the deep dye section of polyamide fibre 6
Method, the preparation method includes following concrete operation step：
(1), material allocation：
Caprolactam is preheated：Solid-state caprolactam is heated into obtain caprolactam melt liquid by melting, the Summer Solstice or the Winter Solstice is laid in
It is standby with groove；
Deep dye additive is prepared：Take terephthalic acid (TPA) and additive TFB-117 and be well mixed, obtain deep dye addition
Agent, it is standby；And the quality of terephthalic acid (TPA) is that caprolactam melts 3~the 4 ‰ of weight, TFB- in gained dye additive deeply
117 quality is that caprolactam melting weight is 8~10 ‰；
Titanium dioxide is prepared：According to the demand to be prepared section species, the titanium dioxide of allotment respective quality concentration is adjusted
It is standby with liquid；
(2), prepolymerization：By gained caprolactam melt liquid, deep dye additive and titanium dioxide seasoning liquid through dynamic
State blender is uniformly mixed, and carries out ring-opening reaction and sudden reaction successively into prepolymerization tower afterwards；And ring-opening reaction temperature is
244~246 DEG C, pre-polymerization pressure is 1450~1550mbarg, and the melt relative viscosity that reaction comes out after terminating from prepolymerization tower is
1.69~1.71；
(3), final polymerization reaction：It is anti-that the melt come out from prepolymerization tower carries out addition polymerization successively through gear pump into final polymerization tower
Should and polycondensation reaction；And the melt temperature control entered after final polymerization tower is at 242~246 DEG C, reaction pressure control 1050~
1100mbara, the melt relative viscosity that reaction comes out after terminating from final polymerization tower is 2.26~2.28；
(4), underwater cutpellet：The melt come out from final polymerization tower is delivered to melt prefilter through gear pump, after filtering
By forming processes formation strip, section is cut into by pelleter after then cooling down under water；
(5), extract：Gained is cut into slices and is placed in extraction tower and with 246 DEG C of the extraction processing that carries out, and water-bath ratio is 1:
1.2~1:1.4；
(6) cooling, is dried：Section after extraction processing is placed in drying tower and is passed through 124~128 DEG C of nitrogen and is done
It is dry, and solid phase of cutting into slices is completed, it is 2.46~2.50 to make the final relative viscosity of section；Dried section is handed over by nitrogen heat
Changing makes its temperature be down to less than 45 DEG C, then gained section is the deep dye section of the polyamide fibre 6.
Further, the preparation method also includes following concrete operation step：(7), section packing：Gained polyamide fibre 6 is deep
Slices synthesis method feed bin is contaminated, and is packaged into by baling press required specification.
The beneficial effects of the present invention are：
A kind of preparation method of the deep dye section of polyamide fibre 6 is provided, cut into slices via the deep dye of polyamide fibre made from preparation method of the present invention 6
With higher heat resistance, deep dye can be applied to, so as to avoid oxidation because can not deeply contaminate and easily occur and yellow
Phenomenon so that product has higher added value, can form higher economic benefit.
【Embodiment】
A kind of preparation method of the deep dye section of polyamide fibre 6 of the present invention, the preparation method includes following concrete operation step：
(1), material allocation：
Caprolactam is preheated：Solid-state caprolactam is heated into obtain caprolactam melt liquid by melting, the Summer Solstice or the Winter Solstice is laid in
It is standby with groove；
Deep dye additive is prepared：Take terephthalic acid (TPA) and additive TFB-117 and be well mixed；Obtain deep dye addition
Agent, it is standby；And the quality of terephthalic acid (TPA) is that caprolactam melts 3~the 4 ‰ of weight, TFB- in gained dye additive deeply
117 quality is that caprolactam melting weight is 8~10 ‰；
Titanium dioxide is prepared：According to the demand to be prepared section species, the titanium dioxide of allotment respective quality concentration is adjusted
It is standby with liquid；Specifically, when preparing semi-dulling chips, allotment mass percent is allocated for 0.3 ± 0.02% titanium dioxide
Liquid；When preparing full-dull polyester, the titanium dioxide seasoning liquid that allotment mass percent is 1.6 ± 0.02%；Preparation has light to cut greatly
During piece, the titanium dioxide seasoning liquid that allotment mass percent is 0%；
(2), prepolymerization：By gained caprolactam melt liquid, deep dye additive and titanium dioxide seasoning liquid through dynamic
State blender is uniformly mixed, and carries out ring-opening reaction and sudden reaction successively into prepolymerization tower afterwards；And ring-opening reaction temperature is
244~246 DEG C, pre-polymerization pressure is 1450~1550mbarg, and the melt relative viscosity that reaction comes out after terminating from prepolymerization tower is
1.69~1.71；
(3), final polymerization reaction：The melt come out from prepolymerization tower through gear pump enter final polymerization tower carry out sudden reaction and
Polycondensation reaction；And the melt temperature control entered after final polymerization tower is at 242~246 DEG C, reaction pressure control 1050~
1100mbara, the melt relative viscosity that reaction comes out after terminating from final polymerization tower is 2.26~2.28；
(4), underwater cutpellet：The melt come out from final polymerization tower is delivered to melt prefilter through gear pump, after filtering
By forming processes formation strip, section is cut into by pelleter after then cooling down under water；
(5), extract：Gained section is placed in extraction tower and extraction processing is carried out with 246 DEG C of water, and water-bath ratio is (i.e.
Section and the volume ratio of extraction hot water used) it is 1:1.2~1:1.4；
(6) cooling, is dried：Section after extraction processing is placed in drying tower and is passed through 124~128 DEG C of nitrogen and is done
It is dry, and solid phase of cutting into slices is completed, it is 2.46~2.50 to make the final relative viscosity of section；Dried section is handed over by nitrogen heat
Changing makes its temperature be down to less than 45 DEG C, then gained section is the deep dye section of the polyamide fibre 6.
It is convenient in order to transport, sell, generally the section of gained is packed, i.e., preparation method may also include following specific
Operating procedure：(7), section packing：By the deep dye slices synthesis method feed bin of gained polyamide fibre 6, and it is packaged into by baling press required rule
Lattice.And it should be noted that during extraction processing, monomer and oligomer are washed in water and made into extraction water is recyclable in section
With section completes its extraction part after extraction and is down to less than 0.5%.
In order to which explanation is further elaborated to a kind of deep preparation method for contaminating section of polyamide fibre 6 of the invention, applicant gives
Specific examples below is gone out.
Embodiment 1
Take solid-state caprolactam and pass it through melting and heat to obtain caprolactam melt liquid, lay in daily groove, it is standby；
Take terephthalic acid (TPA) and additive TFB-117 and be well mixed, obtain deep dye additive (terephthalic acid (TPA) in deep dye additive
Quality be the 4 ‰ of caprolactam melting weight, TFB-117 quality be caprolactam melting weight be 8 ‰), it is standby；
The titanium dioxide seasoning liquid that mass percent is 0.3 ± 0.02% is allocated, it is standby；
Gained caprolactam melt liquid, deep dye additive and titanium dioxide seasoning liquid are uniformly mixed through dynamic mixer
Close, carry out ring-opening reaction and sudden reaction successively into prepolymerization tower afterwards, and ring-opening reaction temperature is 244 DEG C, pre-polymerization pressure
For 1480mbarg, the melt relative viscosity that reaction comes out after terminating from prepolymerization tower is 1.69~1.71；Come out from prepolymerization tower
Melt carry out sudden reaction and polycondensation reaction successively into final polymerization tower through gear pump；And the melt temperature entered after final polymerization tower
Degree control is in 245 DEG C, the melt relative viscosity that reaction pressure control comes out in 1050mbara, reaction after terminating from final polymerization tower
For 2.26~2.28；The melt come out from final polymerization tower is delivered to melt prefilter through gear pump, passes through shaping after filtering
Processing forms strip, and section is cut into by pelleter after then cooling down under water；Gained section is placed in extraction tower and with 246 DEG C
Water carry out extraction processing, and water-bath ratio be 1:1.2；Section after extraction processing is placed in drying tower and is passed through 126 DEG C of nitrogen
It is dried, and completes solid phase of cutting into slices, it is 2.46~2.50 to make the final relative viscosity of section；Dried section passes through nitrogen
Gas heat exchange makes its temperature be down to less than 45 DEG C, then gained section is the deep dye section of semi-dull polyamide fibre 6.
Embodiment 2
Take solid-state caprolactam and pass it through melting and heat to obtain caprolactam molten mass, lay in daily groove, it is standby；Take
Terephthalic acid (TPA) and additive TFB-117 are simultaneously well mixed, and obtain deep dye additive (terephthalic acid (TPA) in deep dye additive
Quality be the 3 ‰ of caprolactam melting weight, TFB-117 quality be caprolactam melting weight be 10 ‰), it is standby
With；The titanium dioxide seasoning liquid that mass percent is 0.1.6 ± 0.02% is allocated, it is standby；
Gained caprolactam melt liquid, deep dye additive and titanium dioxide seasoning liquid are uniformly mixed through dynamic mixer
Close, carry out ring-opening reaction and sudden reaction successively into prepolymerization tower afterwards, and ring-opening reaction temperature is 246 DEG C, pre-polymerization pressure
For 1450mbarg, the melt relative viscosity that reaction comes out after terminating from prepolymerization tower is 1.69~1.71；Come out from prepolymerization tower
Melt carry out sudden reaction and polycondensation reaction successively into final polymerization tower through gear pump；And the melt temperature entered after final polymerization tower
Degree control is in 242 DEG C, the melt relative viscosity that reaction pressure control comes out in 1080mbara, reaction after terminating from final polymerization tower
For 2.26~2.28；The melt come out from final polymerization tower is delivered to melt prefilter through gear pump, passes through shaping after filtering
Processing forms strip, and section is cut into by pelleter after then cooling down under water；Gained section is placed in extraction tower and with 246 DEG C
Water carry out extraction processing, and water-bath ratio be 1:1.4；Section after extraction processing is placed in drying tower and is passed through 124 DEG C of nitrogen
It is dried, and completes solid phase of cutting into slices, it is 2.46~2.50 to make the final relative viscosity of section；Dried section passes through nitrogen
Gas heat exchange makes its temperature be down to less than 45 DEG C, then gained section is full-dull nylon 6 dye section deeply.
Embodiment 3
Take solid-state caprolactam and pass it through melting and heat to obtain caprolactam melt liquid, lay in daily groove, it is standby；
Take terephthalic acid (TPA) and additive TFB-117 and be well mixed, obtain deep dye additive (terephthalic acid (TPA) in deep dye additive
Quality be the 3 ‰ of caprolactam melting weight, TFB-117 quality be caprolactam melting weight be 10 ‰), it is standby
With；
Gained caprolactam melt liquid is uniformly mixed with deep dye additive through dynamic mixer, afterwards into prepolymerization
Tower carries out ring-opening reaction and sudden reaction successively, and ring-opening reaction temperature is 245 DEG C, and pre-polymerization pressure is 1550mbarg, reaction knot
The melt relative viscosity that Shu Houcong prepolymerization towers come out is 1.69~1.71；The melt come out from prepolymerization tower enters through gear pump
Final polymerization tower carries out sudden reaction and polycondensation reaction successively；And the melt temperature entered after final polymerization tower is controlled at 246 DEG C, reaction
Stress control is in 1100mbara, and the melt relative viscosity that reaction comes out after terminating from final polymerization tower is 2.26~2.28；Gather from whole
The melt that conjunction tower comes out is delivered to melt prefilter through gear pump, after filtering by forming processes formation strip, then water
Section is cut into by pelleter after lower cooling；Gained section is placed in extraction tower and extraction processing is carried out with 246 DEG C of water, and
Water-bath ratio is 1:1.3；Section after extraction processing is placed in drying tower and is passed through 128 DEG C of nitrogen and is dried, and completes section
Solid phase, it is 2.46~2.50 to make the final relative viscosity of section；Dried section drops its temperature by nitrogen heat exchange
To less than 45 DEG C, then gained section as has greatly the deep dye section of light polyamide fibre 6.
By the various embodiments described above prepare obtained by the deep dye section of polyamide fibre 6 be measured, it is known that amido value reaches 70~
80mmol/kg；Therefore, the deep dye section of polyamide fibre 6 made from preparation method of the present invention has higher heat resistance, can be applied to
Deep dye, so as to avoid because that can not contaminate and the oxidation easily occurred and the phenomenon of yellow deeply so that product has higher added value,
Higher economic benefit can be formed.
Claims (2)
1. a kind of preparation method of the deep dye section of polyamide fibre 6, it is characterised in that：The preparation method includes following concrete operation step：
(1), material allocation：
Caprolactam is preheated：Solid-state caprolactam is heated into obtain caprolactam molten mass by melting, laid in daily groove, it is standby
With；
Deep dye additive is prepared：Take terephthalic acid (TPA) and additive TFB-117 and be well mixed, obtain deep dye additive, it is standby
With；And the quality of terephthalic acid (TPA) is that caprolactam melts 3~the 4 ‰ of weight, TFB-117 in gained dye additive deeply
Quality is that caprolactam melting weight is 8~10 ‰；
Titanium dioxide is prepared：According to the demand to be prepared section species, the titanium dioxide seasoning liquid of respective quality concentration is allocated,
It is standby；
(2), prepolymerization：Gained caprolactam melt liquid, deep dye additive and titanium dioxide seasoning liquid is mixed through dynamic
Clutch is uniformly mixed, and carries out ring-opening reaction and sudden reaction successively into prepolymerization tower afterwards；And ring-opening reaction temperature be 244~
246 DEG C, pre-polymerization pressure is 1450~1550mbarg, and the melt relative viscosity that reaction comes out after terminating from prepolymerization tower is 1.69
~1.71；
(3), final polymerization reaction：The melt come out from prepolymerization tower through gear pump into final polymerization tower carry out successively sudden reaction and
Polycondensation reaction；And the melt temperature control entered after final polymerization tower is at 242~246 DEG C, reaction pressure control 1050~
1100mbara, the melt relative viscosity that reaction comes out after terminating from final polymerization tower is 2.26~2.28；
(4), underwater cutpellet：The melt come out from final polymerization tower is delivered to melt prefilter through gear pump, passes through after filtering
Forming processes formation strip, section is cut into after then cooling down under water by pelleter；
(5), extract：Gained section is placed in extraction tower and extraction processing is carried out with 246 DEG C of water, and water-bath ratio is 1:1.2
~1:1.4；
(6) cooling, is dried：Section after extraction processing is placed in drying tower and is passed through 124~128 DEG C of nitrogen and is dried, and
Section solid phase is completed, it is 2.46~2.50 to make the final relative viscosity of section；Dried section is made by nitrogen heat exchange
Its temperature is down to less than 45 DEG C, then gained section is the deep dye section of the polyamide fibre 6.
2. the preparation method that a kind of deep dye of polyamide fibre 6 is cut into slices according to claim 1, it is characterised in that：The preparation method is also wrapped
Include following concrete operation step：(7), section packing：By the deep dye slices synthesis method feed bin of gained polyamide fibre 6, and packed by baling press
Into required specification.
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| CN201710245038.9A CN107022076A (en) | 2017-04-14 | 2017-04-14 | A kind of preparation method of the deep dye section of polyamide fibre 6 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108641079A (en) * | 2018-04-08 | 2018-10-12 | 长乐力恒锦纶科技有限公司 | A kind of chinlon 6 section production technology of the full-dull of high bright-coloured and high dullness |
| CN109762162A (en) * | 2018-12-25 | 2019-05-17 | 中国纺织科学研究院有限公司 | Functional polyamide and method for continuous production thereof |
| CN109811423A (en) * | 2018-12-25 | 2019-05-28 | 中国纺织科学研究院有限公司 | Production method of continuous polymerized melt direct spinning functional polyamide fiber and the functional polyamide fiber |
| CN110105563A (en) * | 2019-04-10 | 2019-08-09 | 江苏海阳锦纶新材料有限公司 | A kind of additive agent modified lab scale craft of functional nylon PA6 in-situ polymerization |
| CN114636308A (en) * | 2022-04-01 | 2022-06-17 | 温州邦鹿化工有限公司 | Continuous drying process for high-performance polylactic acid (PLA) slices |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108641079A (en) * | 2018-04-08 | 2018-10-12 | 长乐力恒锦纶科技有限公司 | A kind of chinlon 6 section production technology of the full-dull of high bright-coloured and high dullness |
| CN109762162A (en) * | 2018-12-25 | 2019-05-17 | 中国纺织科学研究院有限公司 | Functional polyamide and method for continuous production thereof |
| CN109811423A (en) * | 2018-12-25 | 2019-05-28 | 中国纺织科学研究院有限公司 | Production method of continuous polymerized melt direct spinning functional polyamide fiber and the functional polyamide fiber |
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| CN109811423B (en) * | 2018-12-25 | 2021-10-26 | 中国纺织科学研究院有限公司 | Production method of continuous polymerization melt direct spinning functional polyamide fiber and functional polyamide fiber |
| CN110105563A (en) * | 2019-04-10 | 2019-08-09 | 江苏海阳锦纶新材料有限公司 | A kind of additive agent modified lab scale craft of functional nylon PA6 in-situ polymerization |
| CN114636308A (en) * | 2022-04-01 | 2022-06-17 | 温州邦鹿化工有限公司 | Continuous drying process for high-performance polylactic acid (PLA) slices |
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Application publication date: 20170808 |