CN105315394A - Environment-friendly foamed polyvinyl chloride paste resin and preparation method of same - Google Patents

Environment-friendly foamed polyvinyl chloride paste resin and preparation method of same Download PDF

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Publication number
CN105315394A
CN105315394A CN201410279741.8A CN201410279741A CN105315394A CN 105315394 A CN105315394 A CN 105315394A CN 201410279741 A CN201410279741 A CN 201410279741A CN 105315394 A CN105315394 A CN 105315394A
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China
Prior art keywords
parts
weight
catalyzer
environment
vinyl chloride
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CN201410279741.8A
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Chinese (zh)
Inventor
范宜军
张岷
俞昉
阮叶萍
宋清清
陈善琴
陆观澍
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Shanghai Chlor Alkali Chemical Co Ltd
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Shanghai Chlor Alkali Chemical Co Ltd
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Priority to CN201410279741.8A priority Critical patent/CN105315394A/en
Publication of CN105315394A publication Critical patent/CN105315394A/en
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  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

The invention discloses environment-friendly foamed polyvinyl chloride paste resin and a preparation method of same. The preparation method comprises the following steps: (1) mixing 500-700 parts by weight of seeds with the following components including, by weight, 11000-13000 parts of water, 4-7 parts of a buffering agent, 0.4-0.8 parts of an activator and 10-14 parts of sodium pyrosulfite; (2) adding a vinyl chloride monomer to carry out a reaction, wherein the feeding speed of the addition of the vinyl chloride monomer is 3500-5000 L/h in the first 20-30 min, the total amount of the vinyl chloride monomer is 11000-14500 parts, and adding continuously a catalyst and an emulsifier when the temperature reaches 50-60 DEG C, wherein the total weight of the catalyst is 1-2 parts by weight and the total weight of the emulsifier is 40-200 parts by weight; and (3) when the pressure is reduced to 50% of the initial pressure, finishing the reaction and adding 50-150 parts by weight of an environment-friendly viscosity reducer to prepare the product. The paste resin is uniform in particle size distribution, is environment-friendly and can be used for producing wallpaper.

Description

Environment-friendly type foamed polyvinyl chloride paste resin and preparation method thereof
Technical field
The present invention relates to the production method of polyvinyl chloride (PVC) paste resin.
Background technology
Polyvinyl chloride (PVC) paste resin is a kind of is starting raw material with monomeric vinyl chloride, and the polymkeric substance under the initiation of initiator, has in every field and apply very widely.
Chloroethylene polymerization is a very complicated process, different proportioning raw materials and preparation technology, to cause the polyvinyl chloride (PVC) paste resin that performance difference is very large, polyvinyl chloride (PVC) paste resin disclosed in Chinese patent CN200810202351, only can be used in the need of production of bottle cap.
Environment-friendly type foamed polyvinyl chloride paste resin is a kind of high-grade resin for foam material, above-mentioned disclosed common polyvinyl chloride (PVC) paste resin, foreign matter content is high, alkylphenol and alkylphenol polyoxyethylene content overproof, as the preparation for foam material, to lead that poisonous and harmful is residual to exceed standard, product export is defective, has influence on domestic sale and the outlet to European Union simultaneously.
Summary of the invention
The object of this invention is to provide a kind of polyvinyl chloride (PVC) paste resin for the PP Pipe Compound that foams and preparation method thereof, to overcome the above-mentioned defect that prior art exists.
Method of the present invention, comprises the steps:
(1) preparation of seed:
10000 ~ 14000 weight parts waters, 11 ~ 16 weight parts are laid particular stress on Sodium Pyrosulfite, 0.5 ~ 1.2 part by weight of catalyst (I), 4 ~ 8 weight part buffer reagents and 0.6 ~ 1.6 weight part activator mix, ageing 0.2 ~ 0.5 hour at 40 ~ 50 DEG C of temperature, then add vinyl chloride monomer continuously to react, controlling temperature of reaction is 45 ~ 55 DEG C;
In first 20 ~ 30 minutes, vinyl chloride monomer feed rate is 3500 ~ 5000L/h, add emulsifying agent and catalyzer (II) continuously simultaneously, emulsifying agent is 55 ~ 75 weight parts, catalyzer (II) is 1 ~ 2 weight part, adds in 600 ~ 720 minutes, when reaction system pressure reaches 50% of initial pressure, add 6 ~ 11 weight part lauryl alcohols, obtain seed;
Vinyl chloride monomer total amount is 10000 ~ 14000 parts;
Described buffer reagent is sodium bicarbonate;
Described activator is Cupric Chloride Solution, and the concentration of Cupric Chloride Solution is 0.1 ~ 1Kg/L;
Described emulsifying agent is selected from sodium lauryl sulfate;
Catalyzer (I) is Potassium Persulphate, and catalyzer (II) is Potassium Persulphate.
(2) preparation of environment-friendly type foamed polyvinyl chloride paste resin:
11000 ~ 13000 weight parts waters, 4 ~ 7 weight part buffer reagents, 0.4 ~ 0.8 weight part activator, 10 ~ 14 weight parts are laid particular stress on seed 500 ~ 700 weight part mixing of Sodium Pyrosulfite and step (1), then vinyl chloride monomer reaction is added, when adding vinyl chloride monomer reaction, in first 20 ~ 30 minutes, feed rate is 3500 ~ 5000L/h, vinyl chloride monomer total amount is 11000 ~ 14500 parts, when temperature reaches 50 ~ 60 DEG C, adds catalyzer and emulsifying agent continuously; The total amount of catalyzer is 1 ~ 2 weight part, and emulsifying agent is 40 ~ 200 weight parts, reacts and terminates, add 50-150 weight part environment-friendly type viscosity-depression agent, obtain product when pressure drop reaches 50% of initial pressure;
Sodium bicarbonate selected by described buffer reagent;
Described activator is selected from Cupric Chloride Solution, and concentration is 0.1 ~ 1Kg/L;
Described catalyzer is Potassium Persulphate;
Described emulsifying agent is sodium lauryl sulfate;
Described environment-friendly type viscosity-depression agent is castor oil polyoxyethylene ether;
Adopt the polyvinyl chloride (PVC) paste resin for the PP Pipe Compound that foams prepared by aforesaid method, particle diameter is 0.2 ~ 2 μm, even particle size distribution, the amount that the present invention adds initial emulsification agent by adjustment controls the ratio of size particles thus obtains the lower product of BShi viscosity, use environment-friendly type viscosity-depression agent to meet the needs of environment-friendly type foamed polyvinyl chloride paste resin production simultaneously, for a kind of environment-friendly type foamed polyvinyl chloride paste resin, may be used for preparing wallpaper.
Embodiment
In embodiment, as being not particularly illustrated, the proportioning of component is weight part.
Embodiment 1
(1) preparation of seed:
By 12500 parts of water, 14 parts lay particular stress on Sodium Pyrosulfite, 0.7 part of catalyzer (I), 6 parts of buffer reagents, the ageing 0.4 hour at 50 DEG C of temperature of the mixture of 0.7 part of activator, then add vinyl chloride monomer continuously to react, controlling temperature of reaction is 48 DEG C;
In first 20 minutes, vinyl chloride monomer feed rate is 4200L/h, and add emulsifying agent and catalyzer (II) continuously, emulsifying agent is 70 parts, and catalyzer (II) is 1.2 parts, adds in 600 minutes simultaneously;
When whole reaction system pressure reaches 50% of initial pressure, add 11 parts of lauryl alcohols, thus obtain seed.Median size is 0.41 μm, and weight solids content is 31.5%.
It is 11000 weight parts that monomer adds total amount;
The concentration of said Cupric Chloride Solution is 0.4Kg/L;
Described buffer reagent is sodium bicarbonate;
Described activator is Cupric Chloride Solution, and the concentration of Cupric Chloride Solution is 0.1Kg/L;
Described emulsifying agent is selected from sodium lauryl sulfate;
Catalyzer (I) is Potassium Persulphate, and catalyzer (II) is Potassium Persulphate.
(2) preparation of environment-friendly type foamed polyvinyl chloride paste resin:
12000 parts of water, 5 parts of buffer reagents, 0.48 activator, 12 parts of seed 530 weight parts of laying particular stress on Sodium Pyrosulfite and step (1) are mixed, then vinyl chloride monomer reaction is added, when adding vinyl chloride monomer reaction, in first 20 minutes, feed rate is 4500L/h, when temperature reaches 56.5 DEG C, add catalyzer and emulsifying agent continuously; The total amount of catalyzer is 1.5 parts, and emulsifying agent is 70 parts, when pressure drop to initial pressure 50% time reaction terminate, add 70 portions of environment-friendly type viscosity-depression agents, obtain product.
It is 13500 weight parts that monomer adds total amount;
The concentration of Cupric Chloride Solution is 0.5Kg/L.
Sodium bicarbonate selected by described buffer reagent;
Described activator is selected from Cupric Chloride Solution, and concentration is 1Kg/L;
Described catalyzer is Potassium Persulphate;
Described emulsifying agent is sodium lauryl sulfate;
Described environment-friendly type viscosity-depression agent is castor oil polyoxyethylene ether;
Adopt Malvern particle instrument to detect, result is as follows:
Particle volume diameter is 5.66 μm, even particle size distribution, percent solids: 45.5%, Ph:7.6 sedimentation degree: 3.
Embodiment 2
(1) preparation of seed:
By 14000 parts of water, 16 parts lay particular stress on Sodium Pyrosulfite, 1.2 parts of catalyzer (I), 8 parts of buffer reagents, the ageing 0.4 hour at 40 DEG C of temperature of the mixture of 1.6 parts of activators, then add vinyl chloride monomer continuously to react, controlling temperature of reaction is 55 DEG C;
In first 30 minutes, vinyl chloride monomer feed rate is 3500L/h, and add emulsifying agent and catalyzer (II) continuously, emulsifying agent is 55 parts, and catalyzer (II) is 2 parts, adds in 720 minutes simultaneously;
When whole reaction system pressure reaches 50% of initial pressure, add 12 parts of lauryl alcohols, thus obtain seed.Median size is 0.446 μm, and weight solids content is 32.3%%.
It is 14000 weight parts that monomer adds total amount;
The concentration of said Cupric Chloride Solution is 0.4Kg/L;
Described buffer reagent is sodium bicarbonate;
Described activator is Cupric Chloride Solution, and the concentration of Cupric Chloride Solution is 1Kg/L;
Described emulsifying agent is selected from sodium lauryl sulfate;
Catalyzer (I) is Potassium Persulphate, and catalyzer (II) is Potassium Persulphate.
(2) preparation of environment-friendly type foamed polyvinyl chloride paste resin:
13000 parts of water, 7 parts of buffer reagents, 0.8 activator, 14 parts of seed 700 weight parts of laying particular stress on Sodium Pyrosulfite and step (1) are mixed, then vinyl chloride monomer reaction is added, when adding vinyl chloride monomer reaction, in first 30 minutes, feed rate is 3500L/h, when temperature reaches 60 DEG C, add catalyzer and emulsifying agent continuously; The total amount of catalyzer is 1 part, and emulsifying agent is 200 parts, when pressure drop to initial pressure 50% time reaction terminate, add 150 portions of environment-friendly type viscosity-depression agents, obtain product.
It is 11000 weight parts that monomer adds total amount;
The concentration of Cupric Chloride Solution is 0.5Kg/L.
Sodium bicarbonate selected by described buffer reagent;
Described activator is selected from Cupric Chloride Solution, and concentration is 0.1Kg/L;
Described catalyzer is Potassium Persulphate;
Described emulsifying agent is sodium lauryl sulfate;
Described environment-friendly type viscosity-depression agent is castor oil polyoxyethylene ether;
Adopt Malvern particle instrument to detect, result is as follows:
Particle volume diameter is 3.52 μm, even particle size distribution, percent solids: 41.3%, Ph:8.2 sedimentation degree: 2.

Claims (5)

1. the preparation method of environment-friendly type foamed polyvinyl chloride paste resin, it is characterized in that, comprise the steps: 11000 ~ 13000 weight parts waters, 4 ~ 7 weight part buffer reagents, 0.4 ~ 0.8 weight part activator, 10 ~ 14 weight parts lay particular stress on seed 500 ~ 700 weight part mixing of Sodium Pyrosulfite and step (1), then vinyl chloride monomer reaction is added, when adding vinyl chloride monomer reaction, in first 20 ~ 30 minutes, feed rate is 3500 ~ 5000L/h, vinyl chloride monomer total amount is 11000 ~ 14500 parts, when temperature reaches 50 ~ 60 DEG C, add catalyzer and emulsifying agent continuously, the total amount of catalyzer is 1 ~ 2 weight part, and emulsifying agent is 40 ~ 200 weight parts, reacts and terminates, add 50-150 weight part environment-friendly type viscosity-depression agent, obtain product when pressure drop reaches 50% of initial pressure.
2. method according to claim 1, it is characterized in that, the preparation method of described seed is as follows: 10000 ~ 14000 weight parts waters, 11 ~ 16 weight parts are laid particular stress on Sodium Pyrosulfite, 0.5 ~ 1.2 part by weight of catalyst (I), 4 ~ 8 weight part buffer reagents and 0.6 ~ 1.6 weight part activator mix, ageing 0.2 ~ 0.5 hour at 40 ~ 50 DEG C of temperature, then add vinyl chloride monomer continuously to react, controlling temperature of reaction is 45 ~ 55 DEG C;
In first 20 ~ 30 minutes, vinyl chloride monomer feed rate is 3500 ~ 5000L/h, add emulsifying agent and catalyzer (II) continuously simultaneously, emulsifying agent is 55 ~ 75 weight parts, catalyzer (II) is 1 ~ 2 weight part, adds in 600 ~ 720 minutes, when reaction system pressure reaches 50% of initial pressure, add 6 ~ 11 weight part lauryl alcohols, obtain seed; Vinyl chloride monomer total amount is 10000 ~ 14000 parts.
3. method according to claim 2, is characterized in that, described buffer reagent is sodium bicarbonate; Described activator is Cupric Chloride Solution, and the concentration of Cupric Chloride Solution is 0.1 ~ 1Kg/L; Described emulsifying agent is selected from sodium lauryl sulfate; Catalyzer (I) is Potassium Persulphate, and catalyzer (II) is Potassium Persulphate.
4. method according to claim 1, is characterized in that, sodium bicarbonate selected by described buffer reagent; Described activator is selected from Cupric Chloride Solution, and concentration is 0.1 ~ 1Kg/L; Described catalyzer is Potassium Persulphate; Described emulsifying agent is sodium lauryl sulfate; Described environment-friendly type viscosity-depression agent is castor oil polyoxyethylene ether.
5. the environment-friendly type foamed polyvinyl chloride paste resin that according to any one of Claims 1 to 4 prepared by method.
CN201410279741.8A 2014-06-20 2014-06-20 Environment-friendly foamed polyvinyl chloride paste resin and preparation method of same Pending CN105315394A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111333758A (en) * 2020-04-03 2020-06-26 唐山三友氯碱有限责任公司 Production method of environment-friendly polyvinyl chloride resin
CN114181336A (en) * 2021-12-16 2022-03-15 安徽天辰化工股份有限公司 Ultra-small particle size PVC seed and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999055745A1 (en) * 1998-04-27 1999-11-04 Evc Technology Ag Polyvinyl chloride, processes for its production, and compositions containing it
CN101205270A (en) * 2007-11-22 2008-06-25 上海氯碱化工股份有限公司 Production method of PVC paste resin for glove material
CN101735358A (en) * 2008-11-06 2010-06-16 上海氯碱化工股份有限公司 Polrvinyl chloride paste resin special for wallpaper and preparation method thereof
CN101735356A (en) * 2008-11-06 2010-06-16 上海氯碱化工股份有限公司 Polyvinyl chloride paste resin used for preparing bottle caps and method for producing same

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1999055745A1 (en) * 1998-04-27 1999-11-04 Evc Technology Ag Polyvinyl chloride, processes for its production, and compositions containing it
CN101205270A (en) * 2007-11-22 2008-06-25 上海氯碱化工股份有限公司 Production method of PVC paste resin for glove material
CN101735358A (en) * 2008-11-06 2010-06-16 上海氯碱化工股份有限公司 Polrvinyl chloride paste resin special for wallpaper and preparation method thereof
CN101735356A (en) * 2008-11-06 2010-06-16 上海氯碱化工股份有限公司 Polyvinyl chloride paste resin used for preparing bottle caps and method for producing same

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111333758A (en) * 2020-04-03 2020-06-26 唐山三友氯碱有限责任公司 Production method of environment-friendly polyvinyl chloride resin
CN114181336A (en) * 2021-12-16 2022-03-15 安徽天辰化工股份有限公司 Ultra-small particle size PVC seed and preparation method thereof

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Application publication date: 20160210