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CN108384281A - A kind of active phosphogypsum micro mist preparation method - Google Patents

A kind of active phosphogypsum micro mist preparation method Download PDF

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Publication number
CN108384281A
CN108384281A CN201810141828.7A CN201810141828A CN108384281A CN 108384281 A CN108384281 A CN 108384281A CN 201810141828 A CN201810141828 A CN 201810141828A CN 108384281 A CN108384281 A CN 108384281A
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China
Prior art keywords
micro mist
phosphogypsum
active
product
coupling agent
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Pending
Application number
CN201810141828.7A
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Chinese (zh)
Inventor
李泽钢
杨永彬
杨步雷
向前勇
王彩红
朱大勇
鲁圣军
何敏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
GUIZHOU KAILIN PHOSPHOGYPSUM UTILIZATION Co Ltd
Guizhou University
Original Assignee
GUIZHOU KAILIN PHOSPHOGYPSUM UTILIZATION Co Ltd
Guizhou University
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Application filed by GUIZHOU KAILIN PHOSPHOGYPSUM UTILIZATION Co Ltd, Guizhou University filed Critical GUIZHOU KAILIN PHOSPHOGYPSUM UTILIZATION Co Ltd
Priority to CN201810141828.7A priority Critical patent/CN108384281A/en
Publication of CN108384281A publication Critical patent/CN108384281A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/025—Calcium sulfates
    • 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
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • 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
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • 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
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • 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
    • C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
    • C08K2003/3045—Sulfates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Catalysts (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a kind of active phosphogypsum micro mist preparation methods, include the following steps：1）Ardealite micro mist is put into calcium oxide in agitating heater and is stirred and evenly mixed, the pH value of mixture is adjusted in alkalinity, obtains A product；2）A product are subjected to heating stirring processing, obtain B product；3）Aluminate coupling agent is added into B product successively, continues heating stirring processing, finally obtains active phosphogypsum micro mist.The present invention has the active phosphogypsum micro mist surface property prepared good, and method of modifying is simple, feature with obvious effects.

Description

A kind of active phosphogypsum micro mist preparation method
Technical field
The present invention relates to a kind of ardealite processing method, especially a kind of active phosphogypsum micro mist preparation method.
Background technology
Ardealite is the solid waste of Phosphate Fertilizer Industry, generally often produces 1 ton of phosphoric acid and about generates 5-6 tons of ardealites, often gives birth to 1 ton of Diammonium phosphate (DAP) of production discharges 2.5-5 tons of ardealites.Currently, no matter external or domestic, the comprehensive utilization ratio of ardealite all compares It is low, it is main to be handled by the way of stockpiling.China's ardealite adds up nearly hundred million tons of discharge capacity, is discharge capacity maximum one in gypsum offscum Kind, the phosphogypsum slag of discharge occupies a large amount of soils, forms slag mountain, seriously pollutes environment.
The yield of ardealite is very big at present, but its utilization rate is very low.The reason for causing ardealite utilization rate low has very much, but Most importantly ardealite surface property is poor, causes its utilization ways relatively simple.By the performance to ardealite micro mist into Row analysis and understanding, this researcher explores a kind of method of modifying of simple, the lower-cost ardealite micro mist of equipment, to change It has been apt to the surface property of ardealite micro mist, and then has expanded the comprehensive Utilization Ways of ardealite.
Invention content
The object of the present invention is to provide a kind of active phosphogypsum micro mist preparation methods.The present invention has the activity prepared Ardealite micro mist surface property is good, and method of modifying is simple, feature with obvious effects.
Technical scheme of the present invention：A kind of active phosphogypsum micro mist preparation method, includes the following steps：
1）Ardealite micro mist is put into calcium oxide in agitating heater and is stirred and evenly mixed, the pH value for adjusting mixture is in alkalinity, Obtain A product；
2）A product are subjected to heating stirring processing, obtain B product；
3）Aluminate coupling agent is added into B product, continues heating stirring processing, finally obtains the modification as PVC fillers Ardealite.
Active phosphogypsum micro mist preparation method above-mentioned, includes the following steps：
1）Ardealite micro mist is put into calcium oxide in agitating heater and is stirred and evenly mixed, the pH value for adjusting mixture is 9-11, Obtain A product；
2）A product are subjected to heating stirring processing, controlled at 110-130 DEG C, heating time 60-80min obtains B product；
3）Aluminate coupling agent is added into B product, continues heating stirring processing, control heating temperature is 80-100 DEG C, is added Thermal agitation 30-50min finally obtains active phosphogypsum micro mist.
Active phosphogypsum micro mist preparation method above-mentioned, the step 1）In, the granularity of ardealite micro mist is that 10-30 is micro- Rice.
Active phosphogypsum micro mist preparation method above-mentioned, the step 1）In, the pH value of mixture is 10.
Active phosphogypsum micro mist preparation method above-mentioned, the step 2）In, whipping temp is 120 DEG C, and mixing time is 70min。
Active phosphogypsum micro mist preparation method above-mentioned, the step 3）In, aluminate coupling agent accounts for the 1.5- of B quality 2.5%。
Active phosphogypsum micro mist preparation method above-mentioned, the step 3）In, aluminate coupling agent is solid.
Active phosphogypsum micro mist preparation method above-mentioned, the step 3）In, with same matter when aluminate coupling agent is added It is added after the industrial alcohol dilution of amount.
Active phosphogypsum micro mist preparation method above-mentioned, the step 3）In, heating temperature is 90 DEG C, and heating time is 40min。
Beneficial effects of the present invention
1, ardealite micro mist is surface-treated by the present invention by the above method, and the surface property of obtained ardealite micro mist obtains To greatly improving, its application in industrial aspect is extended, the utility value of ardealite is improved.Traditional treatment method system For the ardealite micro mist obtained there are agglomeration, 45 microns of testing sieve residue on sieves are typically larger than 3%.Ardealite produced by the present invention is micro- Powder is tested with 45 microns of testing sieves, residue on sieve≤0.3%, activation grade mass fraction >=90%, oil absorption≤69mL/100g, symbol Standardization requirement, the prepared filler that can be used as the plastic products such as PVC, PP use.
2, for method of the invention in processing, equipment requirement is low, simple for process, but the effect reached is clearly.
Specific implementation mode
With reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
The embodiment of the present invention
Embodiment 1：A kind of active phosphogypsum micro mist preparation method, steps are as follows：
1）The ardealite micro mist that granularity is 20 microns is put into calcium oxide in agitating heater and is stirred and evenly mixed, adjustment mixing The pH value of object is 10, obtains A product；
2）A product are subjected to heating stirring processing, controlled at 120 DEG C, heating time 70min obtains B product；
3）The aluminate coupling agent that mass parts are 2% is added into B product, the industry of equal quality when aluminate coupling agent is added Ethyl alcohol dilutes, and continues heating stirring processing, control heating temperature is 90 DEG C, and heating stirring 40min finally obtains active phosphorus Gypsum Fibrosum micropowder.
Embodiment 2：A kind of active phosphogypsum micro mist preparation method, steps are as follows：
1）The ardealite micro mist that granularity is 10 microns is put into calcium oxide in agitating heater and is stirred and evenly mixed, adjustment mixing The pH value of object is 9, obtains A product；
2）A product are subjected to heating stirring processing, controlled at 110 DEG C, heating time 80min obtains B product；
3）The aluminate coupling agent that mass parts are 1.5% is added into B product, the work of equal quality when aluminate coupling agent is added Industry ethyl alcohol dilutes, and continues heating stirring processing, control heating temperature is 80 DEG C, and heating stirring 50min finally obtains activity Ardealite micro mist.
Embodiment 3：A kind of active phosphogypsum micro mist preparation method, steps are as follows：
1）The ardealite micro mist that granularity is 15 microns is put into calcium oxide in agitating heater and is stirred and evenly mixed, adjustment mixing The pH value of object is 9.5, obtains A product；
2）A product are subjected to heating stirring processing, controlled at 115 DEG C, heating time 75min obtains B product；
3）The aluminate coupling agent that mass parts are 1.8% is added into B product, the work of equal quality when aluminate coupling agent is added Industry ethyl alcohol dilutes, and continues heating stirring processing, control heating temperature is 85 DEG C, and heating stirring 35min finally obtains activity Ardealite micro mist.
Embodiment 4：A kind of active phosphogypsum micro mist preparation method, steps are as follows：
1）The ardealite micro mist that granularity is 25 microns is put into calcium oxide in agitating heater and is stirred and evenly mixed, adjustment mixing The pH value of object is 10.5, obtains A product；
2）A product are subjected to heating stirring processing, controlled at 125 DEG C, heating time 65min obtains B product；
3）The aluminate coupling agent that mass parts are 2.2% is added into B product, the work of equal quality when aluminate coupling agent is added Industry ethyl alcohol dilutes, and continues heating stirring processing, control heating temperature is 95 DEG C, and heating stirring 45min finally obtains activity Ardealite micro mist.
Embodiment 5：A kind of active phosphogypsum micro mist preparation method, steps are as follows：
1）The ardealite micro mist that granularity is 30 microns is put into calcium oxide in agitating heater and is stirred and evenly mixed, adjustment mixing The pH value of object is 11, obtains A product；
2）A product are subjected to heating stirring processing, controlled at 130 DEG C, heating time 60min obtains B product；
3）The aluminate coupling agent that mass parts are 2.5% is added into B product, the work of equal quality when aluminate coupling agent is added Industry ethyl alcohol dilutes, and continues heating stirring processing, control heating temperature is 100 DEG C, and heating stirring 30min finally obtains work Property ardealite micro mist.

Claims (9)

1. a kind of active phosphogypsum micro mist preparation method, which is characterized in that include the following steps：
1）Ardealite micro mist is put into calcium oxide in agitating heater and is stirred and evenly mixed, the pH value for adjusting mixture is in alkalinity, Obtain A product；
2）A product are subjected to heating stirring processing, obtain B product；
3）Aluminate coupling agent is added into B product, continues heating stirring processing, finally obtains active phosphogypsum micro mist.
2. active phosphogypsum micro mist preparation method according to claim 1, which is characterized in that include the following steps：
1）Ardealite micro mist is put into calcium oxide in agitating heater and is stirred and evenly mixed, the pH value for adjusting mixture is 9-11, Obtain A product；
2）A product are subjected to heating stirring processing, controlled at 110-130 DEG C, heating time 60-80min obtains B product；
3）Aluminate coupling agent is added into B product, continues heating stirring processing, control heating temperature is 80-100 DEG C, is added Thermal agitation 30-50min finally obtains active phosphogypsum micro mist.
3. active phosphogypsum micro mist preparation method according to claim 1 or 2, it is characterised in that：The step 1）In, phosphorus The granularity of Gypsum Fibrosum micropowder is 10-30 microns.
4. active phosphogypsum micro mist preparation method according to claim 1 or 2, it is characterised in that：The step 1）In, it mixes The pH value for closing object is 10.
5. active phosphogypsum micro mist preparation method according to claim 1 or 2, it is characterised in that：The step 2）In, it stirs It is 120 DEG C to mix temperature, mixing time 70min.
6. active phosphogypsum micro mist preparation method according to claim 1 or 2, it is characterised in that：The step 3）In, aluminium Acid esters coupling agent accounts for the 1.5-2.5% of B quality.
7. active phosphogypsum micro mist preparation method according to claim 1 or 2, it is characterised in that：The step 3）In, aluminium Acid esters coupling agent is solid.
8. active phosphogypsum micro mist preparation method according to claim 1 or 2, it is characterised in that：The step 3）In, aluminium It is added after being diluted with the industrial alcohol of equal quality when acid esters coupling agent is added.
9. active phosphogypsum micro mist preparation method according to claim 1 or 2, it is characterised in that：The step 3）In, add Hot temperature is 90 DEG C, heating time 40min.
CN201810141828.7A 2018-02-11 2018-02-11 A kind of active phosphogypsum micro mist preparation method Pending CN108384281A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111825421A (en) * 2020-07-29 2020-10-27 襄阳市政建设集团有限公司 Preparation method of active phosphogypsum micro powder based on heat insulation material
CN113527911A (en) * 2021-07-22 2021-10-22 贵州大学 Phosphogypsum surface hydroxylation and hydrophobic modification method and phosphogypsum

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101844884A (en) * 2009-03-27 2010-09-29 瓮福（集团）有限责任公司 Hydrophobic phosphogypsum, and preparation method and application thereof
CN104211105A (en) * 2014-09-25 2014-12-17 瓮福（集团）有限责任公司 Ardealite producing method
CN105348862A (en) * 2015-11-29 2016-02-24 贵州开磷集团股份有限公司 Treatment method for phosphogypsum used for PVC (polyvinyl chloride) material production
CN106006696A (en) * 2016-05-12 2016-10-12 贵州开磷磷石膏综合利用有限公司 Fabrication method and application of gypsum micro powder

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101844884A (en) * 2009-03-27 2010-09-29 瓮福（集团）有限责任公司 Hydrophobic phosphogypsum, and preparation method and application thereof
CN104211105A (en) * 2014-09-25 2014-12-17 瓮福（集团）有限责任公司 Ardealite producing method
CN105348862A (en) * 2015-11-29 2016-02-24 贵州开磷集团股份有限公司 Treatment method for phosphogypsum used for PVC (polyvinyl chloride) material production
CN106006696A (en) * 2016-05-12 2016-10-12 贵州开磷磷石膏综合利用有限公司 Fabrication method and application of gypsum micro powder

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111825421A (en) * 2020-07-29 2020-10-27 襄阳市政建设集团有限公司 Preparation method of active phosphogypsum micro powder based on heat insulation material
CN113527911A (en) * 2021-07-22 2021-10-22 贵州大学 Phosphogypsum surface hydroxylation and hydrophobic modification method and phosphogypsum

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