CN107236225A - A kind of preparation method for the flame-proof polyvinyl chloride that methylates - Google Patents
A kind of preparation method for the flame-proof polyvinyl chloride that methylates Download PDFInfo
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- CN107236225A CN107236225A CN201710608885.7A CN201710608885A CN107236225A CN 107236225 A CN107236225 A CN 107236225A CN 201710608885 A CN201710608885 A CN 201710608885A CN 107236225 A CN107236225 A CN 107236225A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers 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; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers 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; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers 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; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation method for the flame-proof polyvinyl chloride that methylates, the present invention passes through crosslinking Treatment, kaolin is effectively combined with polyvinyl chloride, improve the stability_intensity of finished-product material, reduce reunion, the zinc octoate added simultaneously, kaolin etc. can act as good fire retardant performance, improve the combination property of finished-product material.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method for the flame-proof polyvinyl chloride that methylates.
Background technology
Polyvinyl chloride is VCM in initiators such as peroxide, azo-compounds；Or pressed certainly under light, heat effect
The polymer being polymerized by base polymerization reaction mechanism.Ryuron and vinyl chloride copolymer system are referred to as vinyl chloride tree
Fat.PVC is the white powder of impalpable structure, and the degree of branching is smaller, relative density 1.4 or so, 77~90 DEG C of glass transition temperature,
170 DEG C or so start to decompose, and the stability to light and heat is poor, more than 100 DEG C or through long-time exposure in sunshine, will decompose and
Hydrogen chloride is produced, and further autocatalysis is decomposed, and causes discoloration, physical and mechanical properties also declines rapidly, in actual applications
Stabilizer is must be added to improve the stability to light and heat.Industrial PVC molecular weight is general in 50,000~110,000 scopes
It is interior, with larger polydispersity, the reduction of molecular weight with polymerisation temperature and increase；Without definite melting point, 80~85 DEG C of beginnings are soft
Change, 130 DEG C are changed into viscoelastic state, and 160~180 DEG C start to be changed into viscous state；There are preferable mechanical performance, tensile strength 60MPa
Left and right, 5~10kJ/m2 of impact strength；There are excellent dielectric properties.PVC was once the general-purpose plastics of yield maximum in the world, application
Widely.In construction material, industrial product, commodity, flooring laminate, floor tile, artificial leather, tubing, electric wire, packaging
It is widely used in terms of film, bottle, expanded material, encapsulant, fiber.Then in order to improve the mechanical property of polyvinyl chloride
Can, a variety of inorganic additives are often added wherein, then the poor compatibility of inorganic additive and polymer, the group of easily causing
It is poly-, reduce the stability_intensity of finished product.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of flame-proof polyvinyl chloride that methylates
Preparation method.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method for the flame-proof polyvinyl chloride that methylates, comprises the following steps：
(1) sodium stannate of 4-7 parts by weight is taken, in the deionized water for being added to 10-16 times of its weight, is stirred, is added
The PTMG of 2-3 parts by weight, rise temperature is 60-70 DEG C, and insulated and stirred 20-30 minutes adds 0.6-1 weight
The APP of part, stirs to normal temperature, obtains alcohol dispersion liquid；
(2) zinc oxide, the octyl phenyl cyclotetrasiloxane mixing of 24-30 parts by weight of 5-6 parts by weight are taken, at 40-50 DEG C
Lower insulated and stirred 1-2 hours, is added in above-mentioned alcohol dispersion liquid, is sent in reactor, and regulation temperature of reaction kettle is 100-110
DEG C, insulated and stirred 30-40 minutes is discharged, and precipitation is washed in filtering, and air drying obtains fire-retardant siloxanes；
(3) kaolin of 10-17 parts by weight is taken, is calcined 2-3 hours at 600-800 DEG C, fine powder is worn into after cooling, with
In the 2-mercaptobenzimidazole mixing of 0.4-1 parts by weight, the deionized water for being added to 3-4 times of compound weight, 1-2 weight is added
The sorbester p17 of part, stirs, obtains kaolin dispersion liquid；
(4) above-mentioned fire-retardant siloxanes is taken, is added in above-mentioned kaolin dispersion liquid, stirs, 10-12 parts by weight are added dropwise
, the 3-5% sodium peroxide aqueous solution, rise temperature is 50-60 DEG C, and insulated and stirred 20-30 minutes obtains the fire-retardant kaolinite of hydroxylating
Soil；
(5) polyvinyl chloride of 20-30 parts by weight is taken, is mixed with the dimethyl carbonate of 2-4 parts by weight, compound weight is added to
In the 1-METHYLPYRROLIDONE of 1.8-2 times of amount, stir, obtain polyvinyl chloride solution；
(6) polyacrylamide of 1-3 parts by weight is taken, in the deionized water for being added to 10-20 times of its weight, at 80-90 DEG C
Lower insulated and stirred 3-5 minutes, mixes with the fire-retardant kaolin of above-mentioned hydroxylating, stirs, and 10-14 parts by weight, 10- are added dropwise
Ultrasound 2-3 minutes after 12% formalin, completion of dropping, obtain the fire-retardant kaolin dispersion liquid of hydroxylating；
(7) the fire-retardant kaolin dispersion liquid of above-mentioned hydroxylating is taken, mixes, stirs with polyvinyl chloride solution, is sent to anti-
Answer in kettle, add stannous octoate, regulation temperature of reaction kettle is 80-90 DEG C, and insulated and stirred 1-2 hours discharges, and filtering will be precipitated
Dried 1-2 hours at washing, 100-110 DEG C of vacuum, must methylate fire-retardant kaolin cross-linked polrvinyl chloride；
(8) the above-mentioned fire-retardant kaolin cross-linked polrvinyl chloride that methylates, zinc ricinate, 110-140 with 1-2 parts by weight are taken
The polyvinyl chloride mixing of parts by weight, stirs, is sent in extruder, melting extrusion, cooling, produce it is described methylate it is fire-retardant
Polyvinyl chloride.
Advantages of the present invention：
The present invention by by octyl phenyl cyclotetrasiloxane in the alcoholic solution of sodium stannate disperse, then introduce zinc oxide with
Sodium stannate reacts, and obtains the fire-retardant siloxanes of zinc stannate, then mixes, handled by sodium peroxide with kaolin dispersion liquid, obtained
To the fire-retardant kaolin of hydroxylating, then polyvinyl chloride is mixed with dimethyl carbonate, then mixed with the fire-retardant kaolin of hydroxylating, is led to
Formaldehyde treated is crossed, using dimethyl carbonate as the auxiliary agent that methylates, the fire-retardant kaolin cross-linked polrvinyl chloride that methylates is obtained；
Kaolin is effectively combined by crosslinking Treatment, improves the stabilization of finished-product material by the present invention with polyvinyl chloride
Property intensity, reduce reunion, while the zinc octoate added, kaolin etc. can act as good fire retardant performance, improve
The combination property of finished-product material.
Embodiment
Embodiment 1
A kind of preparation method for the flame-proof polyvinyl chloride that methylates, comprises the following steps：
(1) sodium stannate of 7 parts by weight is taken, in the deionized water for being added to 16 times of its weight, is stirred, 3 weight are added
The PTMG of part, rise temperature is 70 DEG C, insulated and stirred 30 minutes, adds the APP of 1 parts by weight, stirring
To normal temperature, alcohol dispersion liquid is obtained；
(2) zinc oxide, the octyl phenyl cyclotetrasiloxane mixing of 30 parts by weight of 6 parts by weight are taken, is incubated and stirs at 50 DEG C
Mix 2 hours, be added in above-mentioned alcohol dispersion liquid, be sent in reactor, regulation temperature of reaction kettle is 110 DEG C, insulated and stirred 40
Minute, discharge, precipitation is washed in filtering, and air drying obtains fire-retardant siloxanes；
(3) kaolin of 17 parts by weight is taken, is calcined 3 hours at 800 DEG C, fine powder is worn into after cooling, the 2- with 1 parts by weight
Mercaptobenzimidazole is mixed, in the deionized water for being added to 4 times of compound weight, adds the sorbester p17 of 2 parts by weight, and stirring is equal
It is even, obtain kaolin dispersion liquid；
(4) above-mentioned fire-retardant siloxanes is taken, is added in above-mentioned kaolin dispersion liquid, stirs, 12 parts by weight of dropwise addition,
The 5% sodium peroxide aqueous solution, rise temperature is 60 DEG C, and insulated and stirred 30 minutes obtains the fire-retardant kaolin of hydroxylating；
(5) polyvinyl chloride of 30 parts by weight is taken, is mixed with the dimethyl carbonate of 4 parts by weight, 2 times of compound weight is added to
1-METHYLPYRROLIDONE in, stir, obtain polyvinyl chloride solution；
(6) polyacrylamide of 3 parts by weight is taken, in the deionized water for being added to 20 times of its weight, is incubated and stirs at 90 DEG C
Mix 5 minutes, mix, stir with the fire-retardant kaolin of above-mentioned hydroxylating, 14 parts by weight, 12% formalin, drop is added dropwise
Ultrasound 3 minutes after finishing are added, the fire-retardant kaolin dispersion liquid of hydroxylating is obtained；
(7) the fire-retardant kaolin dispersion liquid of above-mentioned hydroxylating is taken, mixes, stirs with polyvinyl chloride solution, is sent to anti-
Answer in kettle, add stannous octoate, regulation temperature of reaction kettle is 90 DEG C, and insulated and stirred 2 hours discharges, and precipitation is washed in filtering,
Dried 2 hours at 110 DEG C of vacuum, must methylate fire-retardant kaolin cross-linked polrvinyl chloride；
(8) the above-mentioned fire-retardant kaolin cross-linked polrvinyl chloride that methylates, zinc ricinate, 140 parts by weight with 2 parts by weight are taken
Polyvinyl chloride mixing, stir, be sent in extruder, melting extrusion, cooling produces the fire-retardant polychlorostyrene second that methylates
Alkene.
Embodiment 2
(1) sodium stannate of 4 parts by weight is taken, in the deionized water for being added to 10 times of its weight, is stirred, 2 weight are added
The PTMG of part, rise temperature is 60 DEG C, and insulated and stirred 20 minutes adds the APP of 0.6 parts by weight, stirred
Mix to normal temperature, obtain alcohol dispersion liquid；
(2) zinc oxide, the octyl phenyl cyclotetrasiloxane mixing of 24 parts by weight of 5 parts by weight are taken, is incubated and stirs at 40 DEG C
Mix 1 hour, be added in above-mentioned alcohol dispersion liquid, be sent in reactor, regulation temperature of reaction kettle is 10 DEG C, 30 points of insulated and stirred
Clock, is discharged, and precipitation is washed in filtering, and air drying obtains fire-retardant siloxanes；
(3) kaolin of 10 parts by weight is taken, is calcined 2 hours at 600 DEG C, fine powder is worn into after cooling, with 0.4 parts by weight
2-mercaptobenzimidazole is mixed, in the deionized water for being added to 3 times of compound weight, adds the sorbester p17 of 1 parts by weight, and stirring is equal
It is even, obtain kaolin dispersion liquid；
(4) above-mentioned fire-retardant siloxanes is taken, is added in above-mentioned kaolin dispersion liquid, stirs, 10-12 parts by weight are added dropwise
, the 3-5% sodium peroxide aqueous solution, rise temperature is 50-60 DEG C, and insulated and stirred 20-30 minutes obtains the fire-retardant kaolinite of hydroxylating
Soil；
(5) polyvinyl chloride of 20 parts by weight is taken, is mixed with the dimethyl carbonate of 2 parts by weight, compound weight 1.8 is added to
In 1-METHYLPYRROLIDONE again, stir, obtain polyvinyl chloride solution；
(6) polyacrylamide of 1 parts by weight is taken, in the deionized water for being added to 10 times of its weight, is incubated and stirs at 80 DEG C
Mix 3 minutes, mix, stir with the fire-retardant kaolin of above-mentioned hydroxylating, 10 parts by weight, 10% formalin, drop is added dropwise
Ultrasound 2 minutes after finishing are added, the fire-retardant kaolin dispersion liquid of hydroxylating is obtained；
(7) the fire-retardant kaolin dispersion liquid of above-mentioned hydroxylating is taken, mixes, stirs with polyvinyl chloride solution, is sent to anti-
Answer in kettle, add stannous octoate, regulation temperature of reaction kettle is 80 DEG C, and insulated and stirred 1 hour discharges, and precipitation is washed in filtering,
Dried 1 hour at 100 DEG C of vacuum, must methylate fire-retardant kaolin cross-linked polrvinyl chloride；
(8) the above-mentioned fire-retardant kaolin cross-linked polrvinyl chloride that methylates, zinc ricinate, 110 parts by weight with 1 parts by weight are taken
Polyvinyl chloride mixing, stir, be sent in extruder, melting extrusion, cooling produces the fire-retardant polychlorostyrene second that methylates
Alkene.
Performance test：
The polyvinyl chloride composite materials of the present invention：
Hardness (Shao A) is that 90-92, tensile strength are that 26.1-28MPa, elongation at break are 326.5-340.1%, breach
Impact strength (kJ/m2) it is 9-11；
Traditional polyvinyl chloride：
Hardness (Shao A) is that 70-74, tensile strength are that 15-20MPa, elongation at break are that 230-273%, notch shock are strong
Spend (kJ/m2) it is 6-7.
Claims (1)
1. a kind of preparation method for the flame-proof polyvinyl chloride that methylates, it is characterised in that comprise the following steps：
(1) sodium stannate of 4-7 parts by weight is taken, in the deionized water for being added to 10-16 times of its weight, is stirred, 2-3 weights are added
The PTMG of part is measured, rise temperature is 60-70 DEG C, and insulated and stirred 20-30 minutes adds 0.6-1 parts by weight
APP, stirs to normal temperature, obtains alcohol dispersion liquid；
(2) zinc oxide, the octyl phenyl cyclotetrasiloxane mixing of 24-30 parts by weight of 5-6 parts by weight are taken, is protected at 40-50 DEG C
Temperature stirring 1-2 hours, is added in above-mentioned alcohol dispersion liquid, is sent in reactor, and regulation temperature of reaction kettle is 100-110 DEG C,
Insulated and stirred 30-40 minutes, is discharged, and precipitation is washed in filtering, and air drying obtains fire-retardant siloxanes；
(3) kaolin of 10-17 parts by weight is taken, is calcined 2-3 hours at 600-800 DEG C, fine powder is worn into after cooling, with 0.4-1
In the 2-mercaptobenzimidazole mixing of parts by weight, the deionized water for being added to 3-4 times of compound weight, 1-2 parts by weight are added
Sorbester p17, stirs, and obtains kaolin dispersion liquid；
(4) above-mentioned fire-retardant siloxanes is taken, is added in above-mentioned kaolin dispersion liquid, stirs, dropwise addition 10-12 parts by weight,
The 3-5% sodium peroxide aqueous solution, rise temperature is 50-60 DEG C, and insulated and stirred 20-30 minutes obtains the fire-retardant kaolin of hydroxylating；
(5) polyvinyl chloride of 20-30 parts by weight is taken, is mixed with the dimethyl carbonate of 2-4 parts by weight, compound weight is added to
In 1.8-2 times of 1-METHYLPYRROLIDONE, stir, obtain polyvinyl chloride solution；
(6) polyacrylamide of 1-3 parts by weight is taken, in the deionized water for being added to 10-20 times of its weight, is protected at 80-90 DEG C
Temperature stirring 3-5 minutes, mixes with the fire-retardant kaolin of above-mentioned hydroxylating, stirs, 10-14 parts by weight are added dropwise, 10-12%'s
Ultrasound 2-3 minutes after formalin, completion of dropping, obtain the fire-retardant kaolin dispersion liquid of hydroxylating；
(7) the fire-retardant kaolin dispersion liquid of above-mentioned hydroxylating is taken, mixes, stirs with polyvinyl chloride solution, be sent to reactor
In, stannous octoate is added, regulation temperature of reaction kettle is 80-90 DEG C, and insulated and stirred 1-2 hours discharges, and precipitation is washed in filtering,
Dried 1-2 hours at 100-110 DEG C of vacuum, must methylate fire-retardant kaolin cross-linked polrvinyl chloride；
(8) the above-mentioned fire-retardant kaolin cross-linked polrvinyl chloride that methylates, zinc ricinate, 110-140 weight with 1-2 parts by weight are taken
The polyvinyl chloride mixing of part, stirs, is sent in extruder, melting extrusion, and cooling produces the fire-retardant polychlorostyrene that methylates
Ethene.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710608885.7A CN107236225A (en) | 2017-07-24 | 2017-07-24 | A kind of preparation method for the flame-proof polyvinyl chloride that methylates |
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| CN201710608885.7A CN107236225A (en) | 2017-07-24 | 2017-07-24 | A kind of preparation method for the flame-proof polyvinyl chloride that methylates |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107556664A (en) * | 2017-10-13 | 2018-01-09 | 安徽同利塑胶彩印有限公司 | A kind of polymeric sol modified vinylene chloride plastics material and preparation method thereof |
| CN107915980A (en) * | 2017-11-23 | 2018-04-17 | 清远初曲智能科技有限公司 | A kind of methylolation flame-retardant polycarbonate material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781435A (en) * | 2010-03-02 | 2010-07-21 | 扬州华声电子实业有限公司 | Heat-resisting polyvinyl chloride wire and cable insulation material and preparation method thereof |
| CN104861325A (en) * | 2014-12-24 | 2015-08-26 | 王玉燕 | Nano kaolin modified polyvinyl chloride (PVC) plastic wood composite material and preparation method thereof |
-
2017
- 2017-07-24 CN CN201710608885.7A patent/CN107236225A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101781435A (en) * | 2010-03-02 | 2010-07-21 | 扬州华声电子实业有限公司 | Heat-resisting polyvinyl chloride wire and cable insulation material and preparation method thereof |
| CN104861325A (en) * | 2014-12-24 | 2015-08-26 | 王玉燕 | Nano kaolin modified polyvinyl chloride (PVC) plastic wood composite material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107556664A (en) * | 2017-10-13 | 2018-01-09 | 安徽同利塑胶彩印有限公司 | A kind of polymeric sol modified vinylene chloride plastics material and preparation method thereof |
| CN107915980A (en) * | 2017-11-23 | 2018-04-17 | 清远初曲智能科技有限公司 | A kind of methylolation flame-retardant polycarbonate material and preparation method thereof |
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Application publication date: 20171010 |