CN101735356B - Polyvinyl chloride paste resin used for preparing bottle caps and method for producing same - Google Patents
Polyvinyl chloride paste resin used for preparing bottle caps and method for producing same Download PDFInfo
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- CN101735356B CN101735356B CN 200810202351 CN200810202351A CN101735356B CN 101735356 B CN101735356 B CN 101735356B CN 200810202351 CN200810202351 CN 200810202351 CN 200810202351 A CN200810202351 A CN 200810202351A CN 101735356 B CN101735356 B CN 101735356B
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Abstract
The invention provides polyvinyl chloride paste resin used for preparing bottle caps and a method for producing the same. The method for preparing the polyvinyl chloride paste resin comprises the following steps of: mixing water, an activating agent, sodium metabisulfite and seeds, adding monomers of vinyl chloride into the mixture for reaction, and when the temperature of the mixture is between 44 and 48 DEG C, continuously adding a catalyst until the reaction is ended; and controlling the speed of feeding the remained monomers of vinyl chloride so as to keep the temperature of the reaction system between 41 and 44 DEG C, adding an emulsifying agent when the reaction temperature is between 42 and 44 DEG C, and when the temperature sharply rises and the pressure is unchanged or drops, namely the reaction is ended, adding polyoxyethylene lauric acid ester into the mixture to obtain the finished product, wherein the grain size of the finished product is 0.2 to 1.3mu m, and the distribution of the grain size is uniform. In the method, the polymerization degree is improved by lowering the temperature of the polymerization reaction and the level of residue of the polyvinyl chloride is lowered by prolonging the recovery time, so that the production requirement of the polyvinyl chloride paste resin which is the special material used for producing the bottle caps is met.
Description
Technical field
The present invention relates to the production method of polyvinyl chloride (PVC) paste resin.
Background technology
Polyvinyl chloride (PVC) paste resin, be a kind of be starting raw material with monomer vinylchlorid, the polymkeric substance under the initiation of initiator.In every field application is very widely arranged.
Being used for polymerization process is a very complicated process, and different proportioning raw materials and preparation technology will cause the very big polyvinyl chloride (PVC) paste resin of performance difference, and the polyvinyl chloride (PVC) paste resin that has only can be used in building materials, and what have only can be used in the preparation gloves.
Be used to prepare the polyvinyl chloride (PVC) paste resin of bottle cap, need the higher polymerization degree and lower vinylchlorid residual quantity, and above-mentioned disclosed common polyvinyl chloride (PVC) paste resin, the polymerization degree generally is 1000-1600, the vinylchlorid residual quantity is higher, is generally 5-10mg/kg, can not satisfy the demand.
Summary of the invention
The purpose of this invention is to provide a kind of polyvinyl chloride (PVC) paste resin and production method thereof that is used to prepare bottle cap, to overcome the above-mentioned defective that prior art exists.
Method of the present invention comprises the steps:
(1) preparation of seed:
With the ageing 0.4~0.6 hour under 46~50 ℃ of temperature of the mixture of the catalyzer (I) of laying particular stress on Sodium Pyrosulfite, 0.5~1.0 weight part of the activator Cupric Chloride Solution of the buffer reagent of the water of 10000~12000 weight parts, 4~7 weight parts, 0.4~1.4 weight part, 8~12 weight parts, chlorination reactive vinyl monomer then, temperature of reaction is 48~50 ℃, in preceding 20~30 minutes, feed rate is 3600~4800 weight parts/h, is cooled to 50~51 ℃;
Catalyzer (II) to the reaction that adds 1~3 weight part then continuously finishes, the vinyl chloride monomer that adds surplus simultaneously continuously, the vinyl chloride monomer of surplus add inbound traffics, be 48~53 ℃ with the temperature of control reaction system and be as the criterion, add the emulsifying agent of 60~80 weight parts then, react to temperature sharply rise, pressure is constant or when descending, reaction finishes, and adds the lauryl alcohol of 8~13 weight parts then, obtains seed, particle diameter is 0.35~0.58 μ m, and the weight solids content is 29~36%;
It is 9000~11000 weight parts that monomer adds total amount;
Described buffer reagent is selected from sodium bicarbonate, bicarbonate of ammonia or sodium hydroxide;
Activator is selected from Cupric Chloride Solution, and concentration is 0.1~0.8Kg/L;
Catalyzer (I) and catalyzer (I) are Potassium Persulphate;
Emulsifying agent is sodium lauryl sulfate or dodecyl sulphate potassium;
The present invention obtains the bigger seed of particle diameter by rising ageing temperature and increase digestion time;
(2) preparation of bottle cap PP Pipe Compound:
The water of 12000~14000 weight parts, the activator of 0.6~1.2 weight part, the seed of laying particular stress on Sodium Pyrosulfite and 550~700 weight parts of 8~12 weight parts are mixed, add the vinyl chloride monomer reaction then, in preceding 20~30 minutes, feed rate is 4000~5000 weight parts/h, when temperature reaches 44~48 ℃, add the catalyzer of 1~3 weight part continuously, finish until reaction;
The feed rate of the vinyl chloride monomer of surplus, be 41~44 ℃ with the temperature of controlling reaction system and be as the criterion, when temperature of reaction reaches 42~44 ℃, add the emulsifying agent TETRADECONIC ACID of 40~150 weight parts, when temperature sharply rises, pressure is constant or when descending, reaction finishes, and adds the polyoxyethylene lauric acid fat of 20-50 weight part, obtain product, particle diameter is 0.2~1.3 μ m, and the polymerization degree is 1600~2100, and the vinylchlorid residual quantity is 2~5mg/kg.
It is 13000~15000 weight parts that monomer adds total amount;
Activator is a Cupric Chloride Solution, and concentration is 0.1~1Kg/L;
Catalyzer is ammonium persulphate or Potassium Persulphate;
Emulsifying agent is TETRADECONIC ACID, sodium lauryl sulphate, lauryl alcohol vitriolate of tartar or laurostearic acid;
Term " temperature sharply rises ", refer to when conversion rate of vinyl chloride reaches 70%~80%, because long molecular chain increases and diffusibility descends, and monomer and small molecules chain still have very high diffusibility, chain termination reaction reduces, the automatic hastening phenomenon of reaction occurs, this reaction is thermopositive reaction, so temperature sharply rises.
Adopt the polyvinyl chloride (PVC) paste resin that is used for the bottle cap PP Pipe Compound of method for preparing, particle diameter is 0.2~1.3 μ m, size distribution is even, the present invention improves the product polymerization degree by reducing polymeric reaction temperature, reduce the polyvinyl chloride residual quantity by prolonging recovery time, thereby satisfy the needs of the polyvinyl chloride (PVC) paste resin production of bottle cap PP Pipe Compound.
Embodiment
Embodiment 1
(1) preparation of seed:
With the ageing 0.5 hour under 48 ℃ of temperature of the mixture of the catalyzer of laying particular stress on Sodium Pyrosulfite, the 0.6 weight part-I Potassium Persulphate of the activator Cupric Chloride Solution of the buffer reagent sodium bicarbonate of the water of 12000 weight parts, 5 weight parts, 0.8 weight part, 11 weight parts, chlorination reactive vinyl monomer then, is temperature of reaction? ℃, in preceding 20 minutes, feed rate is 3800 weight parts/h, is cooled to 50 ℃;
Catalyzer-II Potassium Persulphate to the reaction that adds 3 weight parts then continuously finishes, the vinyl chloride monomer that adds surplus simultaneously continuously, the vinyl chloride monomer of surplus add inbound traffics, temperature with the control reaction system is 50 ℃ and is as the criterion, and adds the emulsifying agent sodium lauryl sulfate of 70 weight parts then, react to temperature sharply rise, pressure is constant or when descending, reaction finishes, the lauryl alcohol that adds 10 weight parts then obtains seed, and median size is 0.46 μ m, and the weight solids content is 30%;
It is 11000 weight parts that monomer adds total amount;
The concentration of said Cupric Chloride Solution is 0.5Kg/L;
(2) preparation of bottle cap PP Pipe Compound:
The water of 12000 weight parts, the activator Cupric Chloride Solution of 0.6 weight part, the seed of laying particular stress on Sodium Pyrosulfite and 580 weight parts of 10 weight parts are mixed, add vinyl chloride monomer then, in preceding 20 minutes, feed rate is 4200 weight parts/h, when temperature reaches 45 ℃, add the catalyzer ammonium persulphate of 2 weight parts continuously, finish until reaction;
The feed rate of going into vinyl chloride monomer of surplus, being 42 ℃ with the temperature of controlling reaction system is as the criterion, when temperature of reaction reaches 42 ℃, the emulsifying agent TETRADECONIC ACID that adds 80 weight parts, when temperature sharply rises, pressure is constant or when descending, reaction finishes, the polyoxyethylene lauric acid fat that adds 30 weight parts obtains product;
It is 14000 weight parts that monomer adds total amount;
The concentration of said Cupric Chloride Solution is 0.6Kg/L.
Adopt the WQL particle size analyzer to carry out particle diameter and detect, particle size range is 1.258 (greatly)~0.269 μ m (little), and small-particle is 10.325 with the ratio Nr of macroparticle, and the polymerization degree is 1850, and the vinylchlorid residual quantity is 3mg/kg.
Embodiment 2
(1) preparation of seed:
With the ageing 0.6 hour under 47 ℃ of temperature of the mixture of the catalyzer of laying particular stress on Sodium Pyrosulfite, the 0.7 weight part-I Potassium Persulphate of the activator Cupric Chloride Solution of the buffer reagent sodium bicarbonate of the water of 13000 weight parts, 6 weight parts, 0.9 weight part, 10 weight parts, chlorination reactive vinyl monomer then, is temperature of reaction? ℃, in preceding 30 minutes, feed rate is 4200 weight parts/h, is cooled to 51 ℃;
Catalyzer-II Potassium Persulphate to the reaction that adds 2 weight parts then continuously finishes, the vinyl chloride monomer that adds surplus simultaneously continuously, the vinyl chloride monomer of surplus add inbound traffics, temperature with the control reaction system is 49 ℃ and is as the criterion, and adds the emulsifying agent sodium lauryl sulfate of 70 weight parts then, react to temperature sharply rise, pressure is constant or when descending, reaction finishes, the lauryl alcohol that adds 9 weight parts then obtains seed, and median size is 0.48 μ m, and the weight solids content is 34%;
It is 10000 weight parts that monomer adds total amount;
The concentration of said Cupric Chloride Solution is 0.6Kg/L;
(2) preparation of bottle cap PP Pipe Compound:
The water of 13000 weight parts, the buffer reagent sodium bicarbonate of 5 weight parts, the activator Cupric Chloride Solution of 0.6 weight part, the seed of laying particular stress on Sodium Pyrosulfite and 600 weight parts of 10 weight parts are mixed, add vinyl chloride monomer then, in preceding 30 minutes, feed rate is 4400 weight parts/h, when temperature reaches 43 ℃, add the catalyzer ammonium persulphate of 3 weight parts continuously, finish until reaction;
The feed rate of going into vinyl chloride monomer of surplus, being 43 ℃ with the temperature of controlling reaction system is as the criterion, when temperature of reaction reaches 43 ℃, the emulsifying agent sodium lauryl sulfate that adds 90 weight parts, when temperature sharply rises, pressure is constant or when descending, reaction finishes, the polyoxyethylene lauric acid fat that adds 40 weight parts obtains product;
It is 14500 weight parts that monomer adds total amount;
The concentration of said Cupric Chloride Solution is 0.7Kg/L.
Adopt the WQL particle size analyzer to carry out particle diameter and detect, particle size range is 1.232 (greatly)~0.271 μ m (little), and small-particle is 14.521 with the ratio Nr of macroparticle.The polymerization degree is 1940, and the vinylchlorid residual quantity is 4mg/kg.
Claims (1)
1. be used to prepare the preparation method of the polyvinyl chloride (PVC) paste resin of bottle cap, it is characterized in that, comprise the steps:
With water, activator, lay particular stress on Sodium Pyrosulfite and seed and mix, add the vinyl chloride monomer reaction then, when temperature reaches 44~48 ℃, add catalyzer continuously, finish until reaction;
The feed rate of the vinyl chloride monomer of surplus, being 41~44 ℃ with the temperature of controlling reaction system is as the criterion, when temperature of reaction reaches 42~44 ℃, add emulsifying agent, when temperature sharply rises, pressure is constant or when descending, reaction finishes, and adds polyoxyethylene lauric acid fat, obtains product, the weight part of each component is: 12000~14000 parts in water, 0.6~1.2 part in activator is laid particular stress on 550~700 parts in 8~12 parts of Sodium Pyrosulfites and seed, 1~3 part of catalyzer, it is 13000~15000 parts that monomer adds total amount;
Activator is a Cupric Chloride Solution, and concentration is 0.1~1Kg/L; Catalyzer is ammonium persulphate, bicarbonate of ammonia or sodium hydroxide; Emulsifying agent is TETRADECONIC ACID, sodium lauryl sulfate, lauryl alcohol vitriolate of tartar or laurostearic acid; Described seed is preparation like this:
(1) with water, buffer reagent, activator, mixture ageing 0.4~0.6 hour under 46~50 ℃ of temperature of laying particular stress on Sodium Pyrosulfite, catalyzer (I), chlorination reactive vinyl monomer then, temperature of reaction is 48~50 ℃, in preceding 20~30 minutes, feed rate is 3600~4800 weight parts/h, is cooled to 50~51 ℃;
(2) adding catalyzer (II) to reaction then continuously finishes, the vinyl chloride monomer that adds surplus simultaneously continuously, the vinyl chloride monomer of surplus add inbound traffics, being 48~53 ℃ with the temperature of controlling reaction system is as the criterion, add emulsifying agent then, react to temperature sharply rise, pressure is constant or when descending, reaction finishes, add lauryl alcohol then, obtain seed;
Catalyzer (I) and catalyzer (II) are Potassium Persulphate;
The weight part of each component is:
It is 9000~11000 weight parts that monomer adds total amount, 10000~12000 parts in water, 4~7 parts of buffer reagents, 0.4~1.4 part in activator, lay particular stress on 8~12 parts of Sodium Pyrosulfites, 0.5~1.0 part of catalyzer (I), 1~3 part of catalyzer (II), 60~80 parts of emulsifying agents, 8~13 parts of lauryl alcohols.
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CN101735356B true CN101735356B (en) | 2011-11-23 |
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CN105315394A (en) * | 2014-06-20 | 2016-02-10 | 上海氯碱化工股份有限公司 | Environment-friendly foamed polyvinyl chloride paste resin and preparation method of same |
SG11201804314PA (en) * | 2015-12-02 | 2018-06-28 | Abu Dhabi Polymers Company Ltd Borouge L L C | Hdpe |
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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