CN113980161A - Method for improving production efficiency of polyvinyl chloride composite resin - Google Patents
Method for improving production efficiency of polyvinyl chloride composite resin Download PDFInfo
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- CN113980161A CN113980161A CN202111360984.0A CN202111360984A CN113980161A CN 113980161 A CN113980161 A CN 113980161A CN 202111360984 A CN202111360984 A CN 202111360984A CN 113980161 A CN113980161 A CN 113980161A
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- polyvinyl chloride
- composite resin
- reaction kettle
- chloride composite
- production efficiency
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- 229920000915 polyvinyl chloride Polymers 0.000 title claims abstract description 78
- 239000004800 polyvinyl chloride Substances 0.000 title claims abstract description 78
- 239000000805 composite resin Substances 0.000 title claims abstract description 77
- 238000000034 method Methods 0.000 title claims abstract description 57
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 124
- 239000002105 nanoparticle Substances 0.000 claims abstract description 38
- 238000003756 stirring Methods 0.000 claims abstract description 38
- 239000004816 latex Substances 0.000 claims abstract description 37
- 229920000126 latex Polymers 0.000 claims abstract description 37
- 239000002270 dispersing agent Substances 0.000 claims abstract description 34
- 239000008367 deionised water Substances 0.000 claims abstract description 30
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 25
- 239000003999 initiator Substances 0.000 claims abstract description 18
- 239000011261 inert gas Substances 0.000 claims description 24
- 238000009775 high-speed stirring Methods 0.000 claims description 17
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 16
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 16
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 16
- 239000001099 ammonium carbonate Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 14
- NMOALOSNPWTWRH-UHFFFAOYSA-N tert-butyl 7,7-dimethyloctaneperoxoate Chemical compound CC(C)(C)CCCCCC(=O)OOC(C)(C)C NMOALOSNPWTWRH-UHFFFAOYSA-N 0.000 claims description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 10
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 10
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 10
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 10
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 10
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 10
- ZACVGCNKGYYQHA-UHFFFAOYSA-N 2-ethylhexoxycarbonyloxy 2-ethylhexyl carbonate Chemical compound CCCCC(CC)COC(=O)OOC(=O)OCC(CC)CCCC ZACVGCNKGYYQHA-UHFFFAOYSA-N 0.000 claims description 6
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 5
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 5
- 239000003002 pH adjusting agent Substances 0.000 claims description 2
- 239000003607 modifier Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 21
- 238000002156 mixing Methods 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 9
- 239000000126 substance Substances 0.000 description 9
- 238000007792 addition Methods 0.000 description 8
- 238000005457 optimization Methods 0.000 description 7
- 239000007795 chemical reaction product Substances 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F114/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F114/02—Monomers containing chlorine
- C08F114/04—Monomers containing two carbon atoms
- C08F114/06—Vinyl chloride
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention relates to the technical field of polyvinyl chloride composite resin, in particular to a method for improving the production efficiency of polyvinyl chloride composite resin, which is carried out according to the following steps: firstly, adding the nanoparticle latex, the pH regulator, the vinyl chloride and the deionized water into a reaction kettle, uniformly stirring, then adding the dispersant and the initiator into the reaction kettle, and carrying out polymerization reaction at a certain pressure and temperature to obtain the polyvinyl chloride composite resin. The method has the advantages of simple process, short feeding time and high production efficiency, and compared with the prior art, the polyvinyl chloride composite resin obtained by the method has the same impact resistance, tensile strength and plasticizing effect, and effectively solves the problem of kettle adhesion in the prior polyvinyl chloride composite resin process.
Description
Technical Field
The invention relates to the technical field of polyvinyl chloride composite resin, and discloses a method for improving the production efficiency of polyvinyl chloride composite resin.
Background
The existing process of the polyvinyl chloride composite resin mostly adopts an emulsion-suspension mixing method for production, and the process specifically comprises the following steps: firstly, replacing air in a reaction kettle with inert gas to ensure that the reaction kettle is in an inert gas environment, adding deionized water (below 30 ℃) into the reaction kettle, adding a pH regulator, then adding a dispersing agent into the reaction kettle, adding nano particle latex twice at an interval of 60min, after the two times of addition, adding an initiator into the kettle, stirring and uniformly mixing, keeping the temperature in the reaction kettle below 30 ℃, finally, adding vinyl chloride into the reaction kettle, starting to heat a jacket of the reaction kettle, carrying out polymerization reaction in the reaction kettle at a pressure of 0.5 to 1.2MPa and a temperature of 47 to 70 ℃, and after the polymerization reaction is finished, sequentially discharging, dehydrating and drying reaction products in the reaction kettle to obtain the polyvinyl chloride composite resin.
The existing polyvinyl chloride composite resin has tedious and long process and long time consumption, in the temperature rise process of a reaction kettle, the temperature of the kettle wall is high, nano particle latex can be adhered to the kettle wall of the reaction kettle, the thermal efficiency of the reaction kettle is seriously influenced, and the over-temperature and over-pressure in the reaction process are caused.
Disclosure of Invention
The invention provides a method for improving the production efficiency of polyvinyl chloride composite resin, overcomes the defects of the prior art, and can effectively solve the problem of kettle adhesion in the prior art of the polyvinyl chloride composite resin.
The technical scheme of the invention is realized by the following measures: a method for improving the production efficiency of polyvinyl chloride composite resin is carried out according to the following steps: replacing air in a reaction kettle with inert gas to ensure that the reaction kettle is in an inert gas environment, and sequentially adding the nanoparticle latex and the pH regulator into the reaction kettle to stir at a low speed; secondly, adding vinyl chloride and hot deionized water into the reaction kettle simultaneously to ensure that the temperature in the reaction kettle is between 52 and 75 ℃, and then adding a dispersing agent into the reaction kettle to stir at a high speed until the mixture is fully mixed; thirdly, adding an initiator into a reaction kettle at the pressure of 0.5MPa to 1.2MPa and the temperature of 47 ℃ to 70 ℃ for polymerization reaction to obtain polyvinyl chloride composite resin; wherein, the raw materials comprise the following components in parts by weight: 100 parts of vinyl chloride, 2.3 to 6.0 parts of nano particle latex, 135 to 145 parts of deionized water, 0.1 to 0.2 part of dispersant, 0.018 to 0.120 part of initiator and 0.02 to 0.05 part of pH value regulator.
The following is further optimization or/and improvement of the technical scheme of the invention:
the dispersing agent is formed by mixing polyvinyl alcohol and hydroxypropyl methyl cellulose in a weight ratio of 1.05-1.10: 1.
The initiator is one of di (2-ethylhexyl) peroxydicarbonate and tert-butyl peroxyneodecanoate.
The pH regulator is one of ammonium bicarbonate and sodium bicarbonate.
The feeding time of the first step and the second step is 1.0h to 1.5 h.
In the first step, the low-speed stirring speed is 55rpm to 65 rpm.
In the second step, the high-speed stirring speed is 140rpm to 150 rpm.
Compared with the prior art, the method has the advantages of simple process, short feeding time and high production efficiency, and the obtained polyvinyl chloride composite resin has the same impact resistance, tensile strength and plasticizing effect, and effectively solves the problem of kettle adhesion in the prior polyvinyl chloride composite resin process.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments may be determined according to the technical solutions and practical situations of the present invention. The various chemical reagents and chemicals mentioned in the present invention are all well known and commonly used in the art, unless otherwise specified.
The invention is further described below with reference to the following examples:
example 1: the method for improving the production efficiency of the polyvinyl chloride composite resin is carried out according to the following method: the method comprises the following steps: replacing air in a reaction kettle with inert gas to ensure that the reaction kettle is in an inert gas environment, and sequentially adding the nanoparticle latex and the pH regulator into the reaction kettle to stir at a low speed; secondly, adding vinyl chloride and hot deionized water into the reaction kettle simultaneously to ensure that the temperature in the reaction kettle is between 52 and 75 ℃, and then adding a dispersing agent into the reaction kettle to stir at a high speed until the mixture is fully mixed; thirdly, adding an initiator into a reaction kettle at the pressure of 0.5MPa to 1.2MPa and the temperature of 47 ℃ to 70 ℃ for polymerization reaction to obtain polyvinyl chloride composite resin; wherein, the raw materials comprise the following components in parts by weight: 100 parts of vinyl chloride, 2.3 to 6.0 parts of nano particle latex, 135 to 145 parts of deionized water, 0.1 to 0.2 part of dispersant, 0.018 to 0.120 part of initiator and 0.02 to 0.05 part of pH value regulator.
In the invention, the nano particle latex is the nano particle latex disclosed in the Chinese patent application No. 201710365043.3 and the invention name is nano particle latex, nano particle reinforced and toughened polyvinyl chloride composite resin and a preparation method thereof.
The existing polyvinyl chloride composite resin process comprises the steps of adding deionized water, a pH regulator, a dispersing agent, a nanoparticle latex and an initiator into a reaction kettle, uniformly stirring, controlling the temperature of the reaction kettle to be below 30 ℃, adding vinyl chloride into the reaction kettle, and carrying out polymerization reaction under a certain pressure and temperature, wherein the charging time before the polymerization reaction in the existing process is about 6 hours.
The raw materials are added into a reaction kettle in sequence, the nano particle latex, the pH regulator, the vinyl chloride and the deionized water are added into the reaction kettle, the mixture is stirred and uniformly mixed, then the dispersing agent and the initiator are added into the reaction kettle, and the polymerization reaction is carried out under certain pressure and temperature.
The existing technology of polyvinyl chloride composite resin controls the temperature in a reaction kettle to be below 30 ℃ through deionized water, and the reason is that the feeding time of nano particle latex is too long and the nano particle latex can be demulsified at high temperature, after the raw materials are added, the temperature of a jacket of the reaction kettle needs to be raised, and in the temperature raising process of the reaction kettle, the temperature of the kettle wall is high, and the nano particle latex can be adhered to the kettle wall of the reaction kettle, so that the product quality problem is finally caused.
The invention shortens the feeding time by changing the adding sequence of the raw materials, can simultaneously add chloroethylene and hot deionized water into the reaction kettle, ensures that the temperature in the reaction kettle is 52-75 ℃, is slightly higher than the normal reaction temperature, and the normal reaction temperature is 47-70 ℃, and then adds the dispersing agent and the initiating agent into the reaction kettle to ensure that the temperature during the polymerization reaction is just reduced to the normal reaction temperature, therefore, the invention does not need to heat a reaction kettle jacket, avoids the adhesion of the nano particle latex on the kettle wall, and simultaneously, because of the addition of the dispersing agent and the initiating agent, the temperature of the reaction kettle is slightly reduced to the normal reaction temperature, and avoids the influence of the temperature change on the product quality.
In the invention, the time from the beginning of charging to the beginning of adding the initiator is not less than 1.0 hour, so that the materials are fully stirred, the chloroethylene is dispersed in a liquid drop form, the charging sequence is changed, the charging time is shortened, and finally, the obtained product still has good performance.
Example 2: the method for improving the production efficiency of the polyvinyl chloride composite resin is carried out according to the following method: the method comprises the following steps: replacing air in a reaction kettle with inert gas to ensure that the reaction kettle is in an inert gas environment, and sequentially adding the nanoparticle latex and the pH regulator into the reaction kettle to stir at a low speed; secondly, adding vinyl chloride and hot deionized water into the reaction kettle simultaneously to ensure that the temperature in the reaction kettle is 52 ℃ or 75 ℃, and then adding a dispersing agent into the reaction kettle to carry out high-speed stirring until the mixture is fully mixed; thirdly, adding an initiator into a reaction kettle at the pressure of 0.5MPa or 1.2MPa and the temperature of 47 ℃ or 70 ℃ for polymerization reaction to obtain polyvinyl chloride composite resin; wherein, the raw materials comprise the following components in parts by weight: 100 parts of vinyl chloride, 2.3 parts or 6.0 parts of nanoparticle latex, 135 parts or 145 parts of deionized water, 0.1 part or 0.2 part of dispersant, 0.018 part or 0.120 part of initiator and 0.02 part or 0.05 part of pH value regulator.
Example 3: in the optimization of the above embodiment, the dispersant is a mixture of polyvinyl alcohol and hydroxypropyl methyl cellulose in a weight ratio of 1.05 to 1.10: 1.
Example 4: as optimization of the above embodiment, the initiator is one of di (2-ethylhexyl) peroxydicarbonate and tert-butyl peroxyneodecanoate.
Example 5: as an optimization of the above embodiment, the pH adjusting agent is one of ammonium bicarbonate and sodium bicarbonate.
Example 6: as an optimization of the above examples, the addition times of the first and second steps were between 1.0 and 1.5 h.
Example 7: as an optimization of the above embodiment, in the first step, the low-speed stirring rotation speed is 55rpm to 65 rpm.
Example 8: as an optimization of the above embodiment, in the second step, the high-speed stirring rotation speed is 140rpm to 150 rpm.
Example 9: the method for improving the production efficiency of the polyvinyl chloride composite resin is carried out according to the following method: replacing air in a reaction kettle with inert gas to ensure that the reaction kettle is in an inert gas environment, and sequentially adding the nanoparticle latex and ammonium bicarbonate into the reaction kettle to carry out low-speed stirring, wherein the low-speed stirring rotating speed is 55 rpm; secondly, adding vinyl chloride and hot deionized water into a reaction kettle simultaneously to ensure that the temperature in the reaction kettle is 60 ℃, adding a dispersing agent (formed by mixing polyvinyl alcohol and hydroxypropyl methyl cellulose in a weight ratio of 1.05: 1) into the reaction kettle, and stirring at a high speed until the mixture is fully mixed, wherein the high-speed stirring speed is 145 rpm; thirdly, adding di (2-ethylhexyl) peroxydicarbonate into a reaction kettle at the pressure of 0.82MPa and the temperature of 54.5 ℃ for polymerization reaction to obtain the polyvinyl chloride composite resin, wherein the raw materials comprise the following components in parts by weight: 100 parts of vinyl chloride, 5.0 parts of nano particle latex, 138 parts of deionized water, 0.18 part of dispersing agent, 0.025 part of tert-butyl peroxyneodecanoate and 0.02 part of ammonium bicarbonate, wherein the feeding time of the first step and the second step is 1.0h, and the high-speed stirring rotating speed is 140 rpm.
Example 10: the method for improving the production efficiency of the polyvinyl chloride composite resin is carried out according to the following method: replacing air in a reaction kettle with inert gas to enable the reaction kettle to be in an inert gas environment, and sequentially adding the nanoparticle latex and sodium bicarbonate into the reaction kettle to carry out low-speed stirring, wherein the low-speed stirring rotating speed is 65 rpm; secondly, adding vinyl chloride and hot deionized water into the reaction kettle simultaneously to ensure that the temperature in the reaction kettle is 73 ℃, adding a dispersing agent (formed by mixing polyvinyl alcohol and hydroxypropyl methyl cellulose in a weight ratio of 1.10: 1) into the reaction kettle, and stirring at a high speed until the mixture is fully mixed, wherein the high-speed stirring speed is 150 rpm; thirdly, adding tert-butyl peroxyneodecanoate into a reaction kettle at the pressure of 1.2MPa and the temperature of 68 ℃ for polymerization reaction to obtain the polyvinyl chloride composite resin, wherein the raw materials comprise the following components in parts by weight: 100 parts of chloroethylene, 3.0 parts of nano particle latex, 140 parts of deionized water, 0.12 part of dispersing agent, 0.020 part of tert-butyl peroxyneodecanoate and 0.05 part of sodium bicarbonate, wherein the feeding time of the first step and the second step is 1.5h, and the high-speed stirring rotating speed is 150 rpm.
Example 11: the method for improving the production efficiency of the polyvinyl chloride composite resin is carried out according to the following method: replacing air in a reaction kettle with inert gas to enable the reaction kettle to be in an inert gas environment, and sequentially adding the nanoparticle latex and sodium hydroxide into the reaction kettle to carry out low-speed stirring, wherein the low-speed stirring rotating speed is 60 rpm; secondly, adding vinyl chloride and hot deionized water into the reaction kettle simultaneously to ensure that the temperature in the reaction kettle is 60 ℃, adding a dispersing agent (formed by mixing polyvinyl alcohol and hydroxypropyl methyl cellulose in a weight ratio of 1.07: 1) into the reaction kettle, and stirring at a high speed until the mixture is fully mixed, wherein the high-speed stirring speed is 145 rpm; thirdly, adding di (2-ethylhexyl) peroxydicarbonate into a reaction kettle at the pressure of 0.82MPa and the temperature of 54.5 ℃ for polymerization reaction to obtain the polyvinyl chloride composite resin, wherein the raw materials comprise the following components in parts by weight: 100 parts of vinyl chloride, 6.0 parts of nano particle latex, 145 parts of deionized water, 0.2 part of dispersing agent, 0.030 part of di (2-ethylhexyl) peroxydicarbonate and 0.04 part of ammonium bicarbonate, wherein the feeding time of the first step and the second step is 1.2h, and the high-speed stirring rotating speed is 145 rpm.
The performance indexes of the polyvinyl chloride composite resins prepared in the embodiments 9 to 11 of the present invention all meet the national regulations, and the kettle cleaning frequency of the present invention is also significantly reduced in the process of preparing the polyvinyl chloride composite resin, thereby effectively improving the production efficiency of the reaction kettle.
Comparative example 1: the conventional method for preparing the polyvinyl chloride composite resin is carried out according to the following steps: firstly, replacing air in a reaction kettle with inert gas to ensure that the reaction kettle is in an inert gas environment, adding deionized water (below 30 ℃) into the reaction kettle, adding ammonium bicarbonate under high-speed stirring, then adding a dispersing agent (formed by mixing polyvinyl alcohol and hydroxypropyl methyl cellulose in a weight ratio of 1.07: 1) into the reaction kettle, adding nano particle latex twice at an interval of 60min, adding tert-butyl peroxyneodecanoate into the reaction kettle after the two additions, stirring and mixing uniformly, keeping the temperature of the reaction kettle at 27 ℃, then adding vinyl chloride into the reaction kettle, starting heating a jacket of the reaction kettle, carrying out polymerization reaction in the reaction kettle at a pressure of 0.82MPa and a temperature of 54.5 ℃, discharging, dehydrating and drying reaction products in the reaction kettle in sequence after the polymerization reaction is finished, obtaining the polyvinyl chloride composite resin, wherein the raw materials comprise the following components in parts by weight: 100 parts of vinyl chloride, 5.0 parts of nano particle latex, 138 parts of deionized water, 0.18 part of dispersing agent, 0.025 part of tert-butyl peroxyneodecanoate and 0.02 part of ammonium bicarbonate, wherein the stirring is high-speed stirring at the stirring speed of 140 rpm.
Compared with the polyvinyl chloride composite resin prepared in the embodiment 11 of the invention, the polyvinyl chloride composite resin prepared in the comparative example 1 of the invention has larger difference of physical and chemical index performance, and the whole production process is often unstable and often produces coarse materials.
Comparative example 2: the conventional method for preparing the polyvinyl chloride composite resin is carried out according to the following steps: firstly, replacing air in a reaction kettle with inert gas to ensure that the reaction kettle is in an inert gas environment, adding ammonium bicarbonate and deionized water (below 30 ℃) into the reaction kettle, starting a polymerization kettle for stirring, then sequentially adding a dispersing agent (formed by mixing polyvinyl alcohol and hydroxypropyl methyl cellulose in a weight ratio of 1.07: 1) and nano particle latex into the reaction kettle, stirring uniformly for not less than 70min, then adding tert-butyl peroxyneodecanoate into the polymerization kettle, keeping the temperature in the reaction kettle at 27 ℃, then adding vinyl chloride into the reaction kettle, starting heating a jacket of the reaction kettle, carrying out polymerization reaction in the reaction kettle under the pressure of 0.82MPa and the temperature of 54.5 ℃, discharging, dehydrating and drying reaction products in the reaction kettle in sequence after the polymerization reaction is finished to obtain the polyvinyl chloride composite resin, wherein, the raw materials comprise the following components in parts by weight: 100 parts of vinyl chloride, 5.0 parts of nano particle latex, 138 parts of deionized water, 0.18 part of dispersing agent, 0.025 part of tert-butyl peroxyneodecanoate and 0.02 part of ammonium bicarbonate, wherein the stirring is high-speed stirring at the stirring speed of 140 rpm.
Compared with the process steps of the comparative example 1, the process of the invention has the advantages that the adding sequence of the ammonium bicarbonate and the deionized water is adjusted, the adding of the nano particle latex is changed from fractional addition to one-time feeding, and the stirring time after the nano particle latex is added is increased. Compared with the polyvinyl chloride composite resin prepared in the embodiment 11 of the invention, the polyvinyl chloride composite resin prepared in the comparative example 2 of the invention has larger difference of physical and chemical index performances, particularly larger fluctuation of impact strength performance, and the whole production process is also often unstable and often produces coarse materials.
Comparative example 3: the conventional method for preparing the polyvinyl chloride composite resin is carried out according to the following steps: firstly, replacing air in a reaction kettle with inert gas to enable the reaction kettle to be in an inert gas environment, adding ammonium bicarbonate and deionized water into the reaction kettle, then sequentially adding a dispersing agent (formed by mixing polyvinyl alcohol and hydroxypropyl methyl cellulose in a weight ratio of 1.07: 1), nanoparticle latex and tert-butyl peroxyneodecanoate into the reaction kettle, stirring and uniformly mixing, keeping the temperature in the reaction kettle at 27 ℃, then adding vinyl chloride into the reaction kettle, starting to heat a jacket of the reaction kettle, carrying out polymerization reaction in the reaction kettle at a polymerization kettle pressure of 0.82MPa and a temperature of 54.5 ℃, and after the polymerization reaction is finished, sequentially discharging, dehydrating and drying reaction products in the reaction kettle to obtain the polyvinyl chloride composite resin, wherein the raw materials comprise the following components in parts by weight: 100 parts of vinyl chloride, 5.0 parts of nano particle latex, 138 parts of deionized water, 0.18 part of dispersing agent, 0.025 part of tert-butyl peroxyneodecanoate and 0.02 part of ammonium bicarbonate, wherein the stirring is high-speed stirring at 145 rpm.
Compared with the process steps of the comparative example 2, the process of the invention has the advantages that the stirring speed is increased by 5rpm, and the requirements on the temperature of deionized water and the time after the nano particle latex is added are eliminated in the comparative example 3. Compared with the polyvinyl chloride composite resin prepared in the embodiment 11 of the invention, the polyvinyl chloride composite resin prepared in the comparative example 3 of the invention has no obvious difference in physical and chemical index performance, the whole production process is stable, and the number of kettle cleaning is 3.
Comparative example 4: the conventional method for preparing the polyvinyl chloride composite resin is carried out according to the following steps: firstly, replacing air in a reaction kettle with inert gas to enable the reaction kettle to be in an inert gas environment, adding ammonium bicarbonate and deionized water into the reaction kettle, then sequentially adding nano particle latex and vinyl chloride into the reaction kettle, uniformly stirring, controlling the temperature in the reaction kettle to be about 60 ℃ and slightly higher than the normal reaction temperature, then sequentially adding a dispersing agent (formed by mixing polyvinyl alcohol and hydroxypropyl methyl cellulose in a weight ratio of 1.07: 1) and tert-butyl peroxyneodecanoate into the reaction kettle, uniformly stirring, carrying out polymerization reaction in the reaction kettle under the pressure of 0.82MPa, and after the polymerization reaction is finished, sequentially discharging, dehydrating and drying reaction products in the reaction kettle to obtain the polyvinyl chloride composite resin, wherein the raw materials comprise the following components in parts by weight: 100 parts of vinyl chloride, 5 parts of nano particle latex, 138 parts of deionized water, 0.18 part of dispersing agent, 0.025 part of tert-butyl peroxyneodecanoate and 0.02 part of ammonium bicarbonate, wherein the stirring is high-speed stirring at the speed of 145 rpm.
Comparative example 4 of the present invention compared to the process of comparative example 3, the order of addition of vinyl chloride, dispersant and initiator was adjusted and the temperature of the reactor was increased prior to addition of the dispersant and initiator. The polyvinyl chloride composite resin prepared in comparative example 4 of the present invention was coarse in the discharge, and the order of addition was not feasible.
The polyvinyl chloride composite resins prepared in comparative examples 1 to 4 of the present invention have various performance indexes, and only the polyvinyl chloride composite resin prepared in comparative example 3 can be compared with the polyvinyl chloride composite resin of the present invention in performance. Therefore, the following is a study of the physical and chemical indexes of the polyvinyl chloride composite resin prepared in example 11 of the present invention and the polyvinyl chloride composite resin prepared in comparative example 3 of the present invention, and at the same time, the sticking of the reaction vessel between the polyvinyl chloride composite resin prepared in example 11 of the present invention and the polyvinyl chloride composite resin prepared in comparative example 3 of the present invention is examined.
Test 1: the physical and chemical indexes of the polyvinyl chloride composite resin prepared by the invention are inspected.
The test method comprises the following steps: the physical and chemical indexes of the polyvinyl chloride composite resin prepared in example 11 of the present invention were examined, and the physical and chemical indexes of the polyvinyl chloride composite resin prepared in comparative example 3 of the present invention were compared, including mass fraction of screen residue, apparent density, particle diameter/radial moment, plasticizer absorption of 100g resin, whiteness, impact strength of simple beam, and tensile strength. The impact strength of the simply supported beam is detected according to a measuring method in national standard GB/T1043.1-2008 'measuring of impact performance of plastic simply supported frames', the tensile strength is detected according to a measuring method in GB/T1040.2-2006 'measuring of tensile performance of plastic', and other indexes are detected according to a measuring method in GB/T5761-2018 'suspension method general type polyvinyl chloride resin'.
And (3) test results: the results of physical and chemical indexes are shown in table 1, and it can be seen from table 1 that, after the process flow of the present invention is adopted, the obtained polyvinyl chloride composite resin has particle size/radial moment slightly increased, and other indexes are all within the specified range, and in the practical application of the polyvinyl chloride composite resin, the particle size/radial moment can be adjusted to the level of the existing process by adjusting the input amount of the dispersing agent. Therefore, compared with the prior art, the polyvinyl chloride composite resin obtained by the invention has the same impact resistance, tensile strength and plasticizing effect.
Test 2: the condition of the sticking kettle of the reaction kettle in the process of preparing the polyvinyl chloride composite resin is inspected.
The test method comprises the following steps: for the polyvinyl chloride composite resin prepared in example 11 of the present invention and the polyvinyl chloride composite resin prepared in comparative example 3 of the present invention, the cleaning date of the reaction vessel was recorded during the preparation of the polyvinyl chloride composite resin.
And (3) test results: as shown in table 2, as can be seen from table 2, the process according to comparative example 1 requires cleaning the reactor once after being put into operation for 3 to 4 days, and the process according to example 11 of the present invention requires cleaning the reactor once after being put into operation for 8 to 9 days, which significantly reduces the frequency of cleaning the reactor after the implementation of the present invention compared with the prior art according to comparative example 1, and increases the cleaning time from the prior cleaning time of 3 to the prior cleaning time of 12, thereby effectively improving the production efficiency of the reactor and effectively solving the problem of kettle adhesion existing in the prior art of polyvinyl chloride composite resin.
In conclusion, the process is simple, the feeding time is short, the production efficiency is high, the obtained polyvinyl chloride composite resin has the same impact resistance, tensile strength and plasticizing effect, and the problem of kettle adhesion in the existing polyvinyl chloride composite resin process is effectively solved.
The technical characteristics form an embodiment of the invention, which has strong adaptability and implementation effect, and unnecessary technical characteristics can be increased or decreased according to actual needs to meet the requirements of different situations.
Claims (8)
1. A method for improving the production efficiency of polyvinyl chloride composite resin is characterized by comprising the following steps: replacing air in a reaction kettle with inert gas to ensure that the reaction kettle is in an inert gas environment, and sequentially adding the nanoparticle latex and the pH regulator into the reaction kettle to stir at a low speed; secondly, adding vinyl chloride and hot deionized water into the reaction kettle simultaneously to ensure that the temperature in the reaction kettle is between 52 and 75 ℃, and then adding a dispersing agent into the reaction kettle to stir at a high speed until the mixture is fully mixed; thirdly, adding an initiator into a reaction kettle at the pressure of 0.5MPa to 1.2MPa and the temperature of 47 ℃ to 70 ℃ for polymerization reaction to obtain polyvinyl chloride composite resin; wherein, the raw materials comprise the following components in parts by weight: 100 parts of vinyl chloride, 2.3 to 6.0 parts of nano particle latex, 135 to 145 parts of deionized water, 0.1 to 0.2 part of dispersant, 0.018 to 0.120 part of initiator and 0.02 to 0.05 part of pH value regulator.
2. The method for improving the productivity of polyvinyl chloride composite resin according to claim 1, wherein the dispersing agent is a mixture of polyvinyl alcohol and hydroxypropylmethyl cellulose in a weight ratio of 1.05 to 1.10: 1.
3. The method for improving the production efficiency of polyvinyl chloride composite resin according to claim 1 or 2, wherein the initiator is one of di (2-ethylhexyl) peroxydicarbonate and t-butyl peroxyneodecanoate.
4. The method for improving the production efficiency of polyvinyl chloride composite resin according to claim 1 or 2, wherein the pH adjusting agent is one of ammonium bicarbonate and sodium bicarbonate; or/and the feeding time of the first step and the second step is 1.0h to 1.5 h.
5. The method for improving the production efficiency of polyvinyl chloride composite resin according to claim 3, wherein the ppH modifier is one of ammonium bicarbonate and sodium bicarbonate; or/and the feeding time of the first step and the second step is 1.0h to 1.5 h.
6. The method for improving the production efficiency of polyvinyl chloride composite resin according to claim 1, 2 or 5, wherein in the first step, the low-speed stirring rotation speed is 55rpm to 65 rpm; or/and in the second step, the high-speed stirring speed is 140rpm to 150 rpm.
7. The method for improving the production efficiency of polyvinyl chloride composite resin according to claim 3, wherein in the first step, the low-speed stirring rotation speed is 55rpm to 65 rpm; or/and in the second step, the high-speed stirring speed is 140rpm to 150 rpm.
8. The method for improving the production efficiency of polyvinyl chloride composite resin according to claim 4, wherein in the first step, the low-speed stirring rotation speed is 55rpm to 65 rpm; or/and in the second step, the high-speed stirring speed is 140rpm to 150 rpm.
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| JPH04248809A (en) * | 1991-01-25 | 1992-09-04 | Tosoh Corp | Suspension polymerization of vinyl chloride |
| JPH04248810A (en) * | 1991-01-25 | 1992-09-04 | Tosoh Corp | Suspension polymerization of vinyl chloride |
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| CN106279477A (en) * | 2016-08-08 | 2017-01-04 | 新疆宜化化工有限公司 | The production method of a kind of modified PVC and process units |
| CN107082984A (en) * | 2017-05-22 | 2017-08-22 | 新疆中泰化学股份有限公司 | Nano-particle latex and nano particle reinforced tenacity increased vinyl chloride compound resin and preparation method thereof |
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| JPH04248813A (en) * | 1991-01-25 | 1992-09-04 | Tosoh Corp | Suspension polymerization of vinyl chloride |
| JPH04248809A (en) * | 1991-01-25 | 1992-09-04 | Tosoh Corp | Suspension polymerization of vinyl chloride |
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