CN101735358A - Polrvinyl chloride paste resin special for wallpaper and preparation method thereof - Google Patents
Polrvinyl chloride paste resin special for wallpaper and preparation method thereof Download PDFInfo
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- CN101735358A CN101735358A CN200810202353A CN200810202353A CN101735358A CN 101735358 A CN101735358 A CN 101735358A CN 200810202353 A CN200810202353 A CN 200810202353A CN 200810202353 A CN200810202353 A CN 200810202353A CN 101735358 A CN101735358 A CN 101735358A
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Abstract
The invention provides polrvinyl chloride paste resin special for wallpaper and a preparation method thereof. The preparation method comprises the following steps of: mixing water, a buffering agent, an activating agent, sodium pyrosulfite and a seed with the grain diameter of o.35-0.58 micrometer; then adding a vinyl chloride monomer for reaction; when temperature reaches 55-60 DEG C, continuously adding a catalyst; when reaction temperature reaches 56-58 DEG C, adding an emulsifying agent; and when the temperature is sharply increased and the pressure is unchanged or reduced, and adding a polyoxyethylene octyl phenol ether when the reaction is finished so as to obtain a product. The polrvinyl chloride paste resin special for the wallpaper and prepared by the method has the grain diameter of 0.3-1.5 micrometers and uniform grain diameter distribution, thereby meeting the requirements for the production of the polrvinyl chloride paste resin special for the wallpaper.
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, different proportioning raw materials and preparation technology will cause the very big polyvinyl chloride (PVC) paste resin of performance difference, the disclosed polyvinyl chloride (PVC) paste resin of present patent, only can be used in building materials, and have only can be used in the preparation gloves.
Wallpaper is a kind of high-grade material that is used to decorate, above-mentioned disclosed common polyvinyl chloride (PVC) paste resin, foreign matter content height, BShi viscosity is big, as is used for the preparation of wallpaper, will cause the wallpaper top coat bad, bubble easily, processing characteristics is not good, influences the wallpaper appearance property.
Summary of the invention
The purpose of this invention is to provide a kind of polyvinyl chloride (PVC) paste resin that is used for the wallpaper PP Pipe Compound and preparation method thereof, 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 0.3～0.5 hour under 44～48 ℃ of temperature of the mixture of catalyzer (the I)-Potassium Persulphate of laying particular stress on Sodium Pyrosulfite, 0.6～1.0 weight part of the activator of the buffer reagent of the water of 12000～14000 weight parts, 5～8 weight parts, 0.5～1.5 weight part, 10～15 weight parts, chlorination reactive vinyl monomer then, temperature of reaction is 49～51 ℃, in preceding 20～30 minutes, feed rate is 3500～5000 weight parts/h, is cooled to 50～51 ℃;
Catalyzer (II) Potassium Persulphate to the reaction that adds 1～2 weight part 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 47～52 ℃ and is as the criterion, and adds the emulsifying agent of 50～70 weight parts then, react to temperature sharply rise, pressure is constant or when descending, the lauryl alcohol that adds 7～12 weight parts then, obtain seed, particle diameter is 0.35～0.58 μ m, and the weight solids content is 29～36%;
It is 10000～12000 weight parts that vinyl chloride monomer adds total amount;
Described buffer reagent is selected from a kind of in sodium bicarbonate, bicarbonate of ammonia or the sodium hydroxide;
The preferred Cupric Chloride Solution of described activator, the concentration of Cupric Chloride Solution are 0.1～1Kg/L;
Described emulsifying agent is selected from sodium lauryl sulfate, lauryl alcohol vitriolate of tartar, TETRADECONIC ACID or laurostearic acid.
The present invention obtains the less seed of particle diameter by reducing the ageing temperature and reducing digestion time;
(2) preparation of wallpaper PP Pipe Compound:
Water with 11000～13000 weight parts, the buffer reagent of 4～7 weight parts, 0.4 the activator of～0.8 weight part, seed 500～700 weight parts of laying particular stress on Sodium Pyrosulfite and step (1) of 10～14 weight parts mix, add vinyl chloride monomer then, in preceding 20～30 minutes, feed rate is 3500～5000 weight parts/h, when temperature reaches 55～60 ℃, the catalyzer Potassium Persulphate that adds 1～4 weight part continuously, the feed rate of the vinyl chloride monomer of surplus, being 55～59 ℃ with the temperature of controlling reaction system is as the criterion, when temperature of reaction reaches 56～58 ℃, add the emulsifying agent sodium lauryl sulfate of 40～200 weight parts; When temperature sharply rises, pressure is constant or when descending, reaction finishes, and adds the polyoxyethylene octyl phenol ether of 50-150 weight part;
It is 13000～14500 weight parts that monomer adds total amount;
Buffer reagent is selected from sodium bicarbonate, bicarbonate of ammonia, sodium hydroxide
Activator is selected from Cupric Chloride Solution, and concentration is 0.1～1Kg/L;
Above-mentioned 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 wallpaper PP Pipe Compound of method for preparing, particle diameter is 0.3～1.5 μ m, size distribution is even, thereby the ratio that the present invention controls size particles by the amount that adds initial emulsifying agent obtains the lower product of BShi viscosity, satisfies the needs of the polyvinyl chloride (PVC) paste resin production of wallpaper PP Pipe Compound.
Embodiment
Embodiment 1
(1) preparation of seed:
With the ageing 0.4 hour under 46 ℃ 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, 1.0 weight parts, 12 weight parts, add vinyl chloride monomer then, temperature of reaction is 50 ℃, in preceding 20 minutes, feed rate is 2500 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 50 ℃ and is as the criterion, and adds the emulsifying agent sodium lauryl sulfate of 55 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 0.42 μ m, and the weight solids content is 32%;
It is 11000 weight parts that monomer adds total amount;
The concentration of said Cupric Chloride Solution is 0.4Kg/L;
(2) preparation of wallpaper PP Pipe Compound:
The water of 13000 weight parts, the buffer reagent sodium bicarbonate of 6 weight parts, the activator Cupric Chloride Solution of 0.5 weight part, the seed of laying particular stress on Sodium Pyrosulfite and 530 weight parts of 12 weight parts are mixed, add vinyl chloride monomer then, in preceding 20 minutes, feed rate is 4500 weight parts/h, when temperature reaches 58 ℃, add the catalyzer Potassium Persulphate of 2 weight parts continuously, finish until reaction;
The feed rate of going into vinyl chloride monomer of surplus, being 57 ℃ with the temperature of controlling reaction system is as the criterion, when temperature of reaction reaches 57.5 ℃, the emulsifying agent sodium lauryl sulfate that adds 100 weight parts, when temperature sharply rises, pressure is constant or when descending, reaction finishes, the polyoxyethylene octyl phenol ether that adds 100 weight parts obtains product;
It is 13500 weight parts that monomer adds total amount;
The concentration of said Cupric Chloride Solution is 0.5Kg/L.
Adopt the WQL particle size analyzer to carry out particle diameter and detect, particle size range is 1.421 (greatly)～0.324 μ m (little), and small-particle is 11.857 with the ratio Nr of macroparticle, BShi viscosity 4650, impurity 10.
Embodiment 2
(1) preparation of seed:
With the ageing 0.4 hour under 45 ℃ of temperature of the mixture of the catalyzer of laying particular stress on Sodium Pyrosulfite, the 0.8 weight part-I Potassium Persulphate of the activator Cupric Chloride Solution of the buffer reagent sodium bicarbonate of the water of 14000 weight parts, 5 weight parts, 0.8 weight part, 14 weight parts, add vinyl chloride monomer then, temperature of reaction is 49 ℃, in preceding 30 minutes, feed rate is 4000 weight parts/h, is cooled to 50 ℃;
Catalyzer-II Potassium Persulphate to the reaction that adds 1 weight part 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 60 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 0.40 μ m, and the weight solids content is 33%;
It is 10000 weight parts that monomer adds total amount;
The concentration of said Cupric Chloride Solution is 0.6Kg/L;
(2) preparation of wallpaper PP Pipe Compound:
The water of 12000 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 510 weight parts of 10 weight parts are mixed, add vinyl chloride monomer then, in preceding 30 minutes, feed rate is 4200 weight parts/h, when temperature reaches 57 ℃, add the catalyzer Potassium Persulphate of 3 weight parts continuously, finish until reaction;
The feed rate of going into vinyl chloride monomer of surplus, being 56 ℃ with the temperature of controlling reaction system is as the criterion, when temperature of reaction reaches 57 ℃, the emulsifying agent sodium lauryl sulfate that adds 80 weight parts, when temperature sharply rises, pressure is constant or when descending, reaction finishes, the polyoxyethylene octyl phenol ether that adds 120 weight parts obtains product;
It is 13000 weight parts that monomer adds total amount;
The concentration of Cupric Chloride Solution is 0.6Kg/L.
Adopt the WQL particle size analyzer to carry out particle diameter and detect, particle size range is 1.358 μ m (greatly)～0.389 μ m (little), and small-particle is 16.875 with the ratio Nr of macroparticle, BShi viscosity 4390, impurity 7.
Claims (9)
1. a seed that is used to prepare the polyvinyl chloride (PVC) paste resin of wallpaper special use is characterized in that, is preparation like this:
(1) with water, buffer reagent, activator, mixture ageing 0.3～0.5 hour under 44～48 ℃ of temperature of laying particular stress on Sodium Pyrosulfite, catalyzer (I), chlorination reactive vinyl monomer then, temperature of reaction is 49～51 ℃;
(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 47～52 ℃ 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, add lauryl alcohol then, obtains seed.
2. seed according to claim 1, it is characterized in that, the parts by weight of each component are: 12000～14000 parts in water, 5～8 parts of buffer reagents, 0.5～1.5 part in activator, lay particular stress on 10～15 parts of Sodium Pyrosulfites, 0.6～1.0 part of catalyzer (I), 1～2 part of catalyzer (II), 50～70 parts of emulsifying agents, 7～12 parts of lauryl alcohols, 10000～12000 parts of vinyl chloride monomers.
3. seed according to claim 2 is characterized in that, in the step (1), in preceding 20～30 minutes, the vinyl chloride monomer feed rate is 3500～5000 weight parts/h.
4. seed according to claim 2 is characterized in that, described buffer reagent is selected from a kind of in sodium bicarbonate, bicarbonate of ammonia or the sodium hydroxide; Described activator is a Cupric Chloride Solution, and the concentration of Cupric Chloride Solution is 0.1～1Kg/L; Described emulsifying agent is selected from sodium lauryl sulfate, lauryl alcohol vitriolate of tartar, TETRADECONIC ACID or laurostearic acid, and catalyzer (I) is a Potassium Persulphate, and catalyzer (II) is a Potassium Persulphate.
5. the method for preparing the polyvinyl chloride (PVC) paste resin of wallpaper special use, it is characterized in that, comprise the steps: water, buffer reagent, activator, lay particular stress on Sodium Pyrosulfite and each described seed mixing of claim 1～4, add the vinyl chloride monomer reaction then, when temperature reaches 55～60 ℃, add catalyzer continuously, when temperature of reaction reaches 56～58 ℃, add emulsifying agent; When temperature sharply rises, pressure is constant or when descending, reaction finishes, and adds polyoxyethylene octyl phenol ether, obtains product.
6. method according to claim 5, it is characterized in that, the parts by weight of each component are: 11000～13000 parts in water, 4～7 parts of buffer reagents, 0.4～0.8 part in activator is laid particular stress on 10～14 parts of Sodium Pyrosulfites, 500～700 parts in seed, 40～200 parts of emulsifying agents, polyoxyethylene octyl phenol ether 50-150 part, 13000～14500 parts of monomers.
7. method according to claim 5, it is characterized in that, when adding the vinyl chloride monomer reaction, in preceding 20～30 minutes, feed rate is 3500～5000 weight parts/h, when temperature reaches 55～60 ℃, add catalyzer continuously, the feed rate of the vinyl chloride monomer of surplus is 55～59 ℃ with the temperature of controlling reaction system and is as the criterion, when temperature of reaction reaches 56～58 ℃, add emulsifying agent; When temperature sharply rises, pressure is constant or when descending, reaction finishes, and adds polyoxyethylene octyl phenol ether.
8. method according to claim 5 is characterized in that buffer reagent is selected from sodium bicarbonate, bicarbonate of ammonia or sodium hydroxide; Activator is selected from Cupric Chloride Solution, and concentration is 0.1～1Kg/L; Catalyzer is a Potassium Persulphate, and emulsifying agent is sodium lauryl sulfate, lauryl alcohol vitriolate of tartar, TETRADECONIC ACID or laurostearic acid.
9. adopt the polyvinyl chloride (PVC) paste resin of the wallpaper special use of each described method preparation of claim 5～9.
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| CN200810202353A CN101735358A (en) | 2008-11-06 | 2008-11-06 | Polrvinyl chloride paste resin special for wallpaper and preparation method thereof |
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| CN200810202353A CN101735358A (en) | 2008-11-06 | 2008-11-06 | Polrvinyl chloride paste resin special for wallpaper and preparation method thereof |
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| CN101735358A true CN101735358A (en) | 2010-06-16 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110862474A (en) * | 2019-11-08 | 2020-03-06 | 上海氯碱化工股份有限公司 | Low-atomization-value polyvinyl chloride paste resin and production method thereof |
-
2008
- 2008-11-06 CN CN200810202353A patent/CN101735358A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110862474A (en) * | 2019-11-08 | 2020-03-06 | 上海氯碱化工股份有限公司 | Low-atomization-value polyvinyl chloride paste resin and production method thereof |
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Open date: 20100616 |