CN100398569C - Method of producing chlorinated polypropylene by water phase suspension method - Google Patents
Method of producing chlorinated polypropylene by water phase suspension method Download PDFInfo
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- CN100398569C CN100398569C CNB200510062019XA CN200510062019A CN100398569C CN 100398569 C CN100398569 C CN 100398569C CN B200510062019X A CNB200510062019X A CN B200510062019XA CN 200510062019 A CN200510062019 A CN 200510062019A CN 100398569 C CN100398569 C CN 100398569C
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- polypropylene
- chlorinated polypropylene
- water
- phase suspension
- water phase
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- -1 polypropylene Polymers 0.000 title claims abstract description 67
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 62
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000000725 suspension Substances 0.000 title claims abstract description 13
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 16
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000460 chlorine Substances 0.000 claims abstract description 14
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 8
- 230000018044 dehydration Effects 0.000 claims abstract description 6
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 6
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000005469 granulation Methods 0.000 claims abstract description 3
- 230000003179 granulation Effects 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 230000008961 swelling Effects 0.000 claims description 13
- 239000003999 initiator Substances 0.000 claims description 7
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 5
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 5
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical group C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000001746 injection moulding Methods 0.000 claims description 2
- 239000002736 nonionic surfactant Substances 0.000 claims description 2
- 229920000193 polymethacrylate Polymers 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 238000007639 printing Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000003063 flame retardant Substances 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 230000000977 initiatory effect Effects 0.000 abstract 1
- 238000002347 injection Methods 0.000 abstract 1
- 239000007924 injection Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 239000010409 thin film Substances 0.000 abstract 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The present invention discloses a method for producing chlorinated polypropylene by a water phase suspension method. First, polypropylene or chlorinated polypropylene is swelled by an organic solvent. Then, swelled polypropylene particles are put in a reaction vessel containing an emulsifying agent, a dispersant, an initiating agent and water, and are in a suspension state under stirring action. Chlorine gas is led into the reaction vessel for chlorination reaction after temperature rise. Further more, chlorinated polypropylene samples with the chlorine content of 15 to 60% are produced through water washing deacidification, neutralization, dehydration, injection granulation and desiccation. The method of the present invention is carried out in a hermetic container. The chlorination reaction process is completed by the chlorination of the reaction vessel in a water phase suspension state. Therefore, the present invention has the advantages of little environmental pollution, short period of chlorination reaction, convenient operation and controllable chlorine content, and can bring great economic effect. The chlorinated polypropylene produced by the technology can be used as a raw material in the industry of a flame retardant, a corrosion-proof coating, a chlorinated rubber substitute, printing ink, an adhesive, a blown thin-film additive, etc.
Description
Technical field
The present invention relates to a kind of water phase suspension and produce the method for Chlorinated Polypropylene III.
Background technology
That Chlorinated Polypropylene III has is nontoxic, acidproof, water-fast, good, the easy film forming of the transparency, characteristics such as nonflammable.According to the difference of cl content, fusing point is generally at 80～160 ℃, and 180～200 ℃ of decomposition temperatures except that being insoluble to alcohol, aliphatic hydrocarbon, can be dissolved in multiple solvents such as aromatic hydrocarbons, ester class, ketone and hydrochloric ether.Chloride massfraction is 63～67% high chlorinated isotactic polypropylene, mainly as the substitute of chlorinated rubber, can be used for the fire retardant and the softening agent of impregnating material, paint adhesion agent and product of rubber and plastic; Chloride massfraction is that 20～40% low chlorinated isotactic polypropylene is mainly as good printing ink vehicle and tackiness agent, the precoated layer of coating, polypropylene film heat-sealing that also is widely used in compound oil ink, the polypropylene injection-molded item of BiOriented Polypropylene Films (BOPP) printing to be to improve the undercoat of heat sealability, polypropene pressure sensitive adhesive band, also can be used as the tackiness agent of the soft properties-correcting agent of sealing agent, polypropylene fibre of properties-correcting agent, the polypropylene pipe joint of polymkeric substance such as polypropylene and polypropylene/Al paper tinsel, polypropylene, polyethylene composite membrane etc.
At present, Chlorinated Polypropylene III is many to be made by chloride solution, and the product chlorination is even, superior performance.But consume fluorochlorohydrocarbon classes such as a large amount of tetracol phenixin in producing, this class material will cause damage to ozonosphere, does not therefore have the solid phase method of fluorochlorohydrocarbon class such as tetracol phenixin and the direction that water phase suspension is important research.Because the heat-transfer capability of solid phase method is relatively poor, the product chlorination is inhomogeneous and have problem such as product coking and can not extensively adopt.The water method is a kind of eco-friendly technology, and polypropylene carries out the chlorating novel process again through swelling earlier and do not appear in the newspapers as yet both at home and abroad.
Summary of the invention
The object of the present invention is to provide a kind of water phase suspension to produce the method for Chlorinated Polypropylene III, is earlier polypropylene to be carried out the chlorating method again through swelling earlier.Chlorination reaction process is that chlorination is finished under the aqueous-phase suspending state of a reactor.
The technical solution adopted for the present invention to solve the technical problems is that the step of this method is as follows: polypropylene or Chlorinated Polypropylene III at first carried out swelling 24～48 hours with organic solvent, then the good polypropylene particles of swelling is put into the emulsifying agent of adding, dispersion agent, initiator is respectively 1.5% of pp material weight, 4.0%, 2% and the reactor of 20～30 times of water of polypropylene weight in, under stirring action, make polypropylene particles be suspended state, heat temperature raising to 60～70 ℃, logical chlorine carries out chlorination reaction, the amount of chlorine that feeds is 0.6～6 times of polypropylene particles weight, be incubated 2 hours, drive remaining chlorine in the still away with air then, chlorizate is through the washing depickling, neutralization, dehydration, the injection moulding granulation, after the drying, can make chlorinity and be 15～60% Chlorinated Polypropylene III sample.
Described polypropylene is that isotatic polypropylene, its melt flow rate (MFR) are 19～27, and polyacrylic granularity is 40～120 orders.
Described organic solvent is a tetracol phenixin.
Described emulsifying agent is the non-ionic surfactant polyoxyethylene alkylphenol; Dispersion agent is a sodium polymethacrylate; Initiator is a benzoyl peroxide.
Described water is for filtering back clean process water, deionized water or distilled water.
The Chlorinated Polypropylene III that the present invention produced, its cl content between 15%-65%, and can be in organic solvents such as tetracol phenixin, dimethylbenzene fully dissolving, solution is clarification, no suspended substance and throw out.
The beneficial effect that the present invention has is: the swelling process of polypropylene particles of the present invention carries out in encloses container, chlorination reaction process is that chlorination is finished under the aqueous-phase suspending state of same reactor, little to environmental pollution on every side, and the chlorination reaction cycle is short, be convenient to operation, cl content and controlled can bring considerable economic.The raw material that can be used as industries such as fire retardant, protective system, chlorinated rubber substitute, printing ink, tackiness agent and blown film additive with the Chlorinated Polypropylene III of this explained hereafter.
Embodiment
Embodiment 1:
At first in an encloses container, add tetracol phenixin and isotatic polypropylene particle, swelling 24h; 2 kilograms of polypropylene particles after the swelling, Disperser Polysodium Methacrylate 80g, emulsifier polyoxyethylene alkylphenol 30g, initiator benzoyl peroxide 40g join in the 50L reactor that fills 30L water, under agitation heat up gradually, be heated to 60 ℃, logical chlorine carries out chlorination reaction, insulation 2h, stop heating afterwards, drive chlorine in the still away with uncontaminated air, chlorizate is through processes such as washing depickling, neutralization, dehydration, dryings, can make chlorinity and be 34.4% Chlorinated Polypropylene III sample I.
Embodiment 2:
Get 2 kilograms in Chlorinated Polypropylene III sample in the example 1, with tetracol phenixin swelling 24h; Chlorinated Polypropylene III sample after the swelling joins in the 50L reactor that fills 30L water, adds Disperser Polysodium Methacrylate 80g, emulsifier polyoxyethylene alkylphenol 30g, initiator benzoyl peroxide 40g afterwards again in reactor; The capping still under agitation is warming up to 60 ℃ gradually, and logical chlorine carries out chlorination reaction, insulation 2h; Stop heating, drive chlorine in the still away with uncontaminated air, chlorizate is through processes such as washing depickling, neutralization, dehydration, dryings, can make chlorinity and be 52.2% Chlorinated Polypropylene III sample II.
Embodiment 3:
Get 2 kilograms in Chlorinated Polypropylene III sample in the example 2, with tetracol phenixin swelling 24h; Chlorinated Polypropylene III sample after the swelling joins in the 50L reactor that fills 30L water, adds Disperser Polysodium Methacrylate 80g, emulsifier polyoxyethylene alkylphenol 30g, initiator benzoyl peroxide 40g afterwards again in reactor; The capping still under agitation is warming up to 60 ℃ gradually, and logical chlorine carries out chlorination reaction, insulation 2h; Stop heating, drive chlorine in the still away with uncontaminated air, chlorizate is through processes such as washing depickling, neutralization, dehydration, dryings, can make chlorinity and be 58.8% Chlorinated Polypropylene III sample III.Get the Chlorinated Polypropylene III sample III0.5 gram among the embodiment 3, under 80 ℃, be dissolved in rapidly in the dimethylbenzene of 20ml and form transparent settled solution, do not have throw out to occur after the cooling.
Claims (5)
1. water phase suspension is produced the method for Chlorinated Polypropylene III, the step that it is characterized in that this method is as follows: polypropylene or Chlorinated Polypropylene III at first carried out swelling 24～48 hours with organic solvent, then the good polypropylene particles of swelling is put into the emulsifying agent of adding, dispersion agent, initiator is respectively 1.5% of polypropylene particles weight, 4.0%, 2% and the reactor of 20～30 times of water of polypropylene particles weight in, under stirring action, make polypropylene particles be suspended state, heat temperature raising to 60～70 ℃, logical chlorine carries out chlorination reaction, the amount of chlorine that feeds is 0.6～6 times of polypropylene particles weight, be incubated 2 hours, drive remaining chlorine in the still away with air then, chlorizate is through the washing depickling, neutralization, dehydration, the injection moulding granulation, after the drying, can make chlorinity and be 15～60% Chlorinated Polypropylene III sample.
2. water phase suspension according to claim 1 is produced the method for Chlorinated Polypropylene III, and it is characterized in that: described polypropylene particles is that isotatic polypropylene, its melt flow rate (MFR) are 19～27, and polyacrylic granularity is 40～120 orders.
3. water phase suspension according to claim 1 is produced the method for Chlorinated Polypropylene III, and it is characterized in that: described organic solvent is a tetracol phenixin.
4. water phase suspension according to claim 1 is produced the method for Chlorinated Polypropylene III, and it is characterized in that: described emulsifying agent is the non-ionic surfactant polyoxyethylene alkylphenol; Dispersion agent is a sodium polymethacrylate; Initiator is a benzoyl peroxide.
5. water phase suspension according to claim 1 is produced the method for Chlorinated Polypropylene III, it is characterized in that: described water is for filtering back clean process water, deionized water or distilled water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510062019XA CN100398569C (en) | 2005-12-15 | 2005-12-15 | Method of producing chlorinated polypropylene by water phase suspension method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510062019XA CN100398569C (en) | 2005-12-15 | 2005-12-15 | Method of producing chlorinated polypropylene by water phase suspension method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1786037A CN1786037A (en) | 2006-06-14 |
| CN100398569C true CN100398569C (en) | 2008-07-02 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200510062019XA Active CN100398569C (en) | 2005-12-15 | 2005-12-15 | Method of producing chlorinated polypropylene by water phase suspension method |
Country Status (1)
| Country | Link |
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| CN (1) | CN100398569C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504059A (en) * | 2011-10-26 | 2012-06-20 | 上海氯碱化工股份有限公司 | Aqueous-phase suspension chlorination method for producing chlorinated polypropylene |
| CN104311708B (en) * | 2014-10-30 | 2016-08-17 | 徐晨曦 | A kind of method that acid phase emulsion fusion method prepares chlorination metallocene polypropylene |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB882524A (en) * | 1956-03-03 | 1961-11-15 | Hoechst Ag | Manufacture of chlorinated polyethylene |
| US4524189A (en) * | 1984-03-20 | 1985-06-18 | The Dow Chemical Company | Preparation of chlorinated polyolefins |
| CN1394885A (en) * | 2001-07-08 | 2003-02-05 | 汪立波 | Industrial production method of chlorinated polypropylene by adopting water phase suspension method and its product. |
-
2005
- 2005-12-15 CN CNB200510062019XA patent/CN100398569C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB882524A (en) * | 1956-03-03 | 1961-11-15 | Hoechst Ag | Manufacture of chlorinated polyethylene |
| US4524189A (en) * | 1984-03-20 | 1985-06-18 | The Dow Chemical Company | Preparation of chlorinated polyolefins |
| CN1394885A (en) * | 2001-07-08 | 2003-02-05 | 汪立波 | Industrial production method of chlorinated polypropylene by adopting water phase suspension method and its product. |
Non-Patent Citations (4)
| Title |
|---|
| 氯化聚丙烯的合成技术进展. 何勇，刘海龙，刘晖.中国氯碱，第12期. 2003 |
| 氯化聚丙烯的合成技术进展. 何勇，刘海龙，刘晖.中国氯碱，第12期. 2003 * |
| 等规聚丙烯水相氯化反应动力学研究. 宋秋生，马海红，边侠玲，徐汝云，徐卫兵.合肥工业大学学报，第28卷第3期. 2005 |
| 等规聚丙烯水相氯化反应动力学研究. 宋秋生，马海红，边侠玲，徐汝云，徐卫兵.合肥工业大学学报，第28卷第3期. 2005 * |
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| Publication number | Publication date |
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| CN1786037A (en) | 2006-06-14 |
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Assignee: Zhejiang University Assignor: Fenghua Yuron Chemical Industry Material Co., Ltd. Contract record no.: 2010330002113 Denomination of invention: Method of producing chlorinated polypropylene by water phase suspension method Granted publication date: 20080702 License type: Exclusive License Open date: 20060614 Record date: 20101102 |
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| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Fenghua Yuron Chemical Industry Material Co., Ltd. Assignor: Zhejiang University Contract record no.: 2010330002113 Denomination of invention: Method of producing chlorinated polypropylene by water phase suspension method Granted publication date: 20080702 License type: Exclusive License Open date: 20060614 Record date: 20101102 |