CN108084318A - A kind of nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride and its manufacturing method - Google Patents
A kind of nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride and its manufacturing method Download PDFInfo
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- CN108084318A CN108084318A CN201711498059.8A CN201711498059A CN108084318A CN 108084318 A CN108084318 A CN 108084318A CN 201711498059 A CN201711498059 A CN 201711498059A CN 108084318 A CN108084318 A CN 108084318A
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- 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
- C08F214/00—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
- C08F214/02—Monomers containing chlorine
- C08F214/04—Monomers containing two carbon atoms
- C08F214/06—Vinyl chloride
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- 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
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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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
- C08K5/00—Use of organic ingredients
- C08K5/0091—Complexes with metal-heteroatom-bonds
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- 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
- C08F222/00—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 carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/36—Amides or imides
- C08F222/38—Amides
- C08F222/385—Monomers containing two or more (meth)acrylamide groups, e.g. N,N'-methylenebisacrylamide
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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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)
- Fireproofing Substances (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride and its manufacturing methods, the nuisanceless flame-resistant high-temperature-resistant Production of PVC raw material include hydrogen chloride, ethylene, oxygen, double (3,5 di-t-butyl, 4 benzylphosphonic acid mono ethyl ester) 5 parts 8 parts of nickel, 5 parts 8 parts of magnesium hydroxide, 3 parts 5 parts of benzoic ether, 3 parts 5 parts of sodium soap, 3 parts 5 parts of niter cake, 5 parts of N N ' methylene-bisacrylamides by weight.The nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride chemical property of the present invention is stable, anti-aging property is strong, light sensitivity is low, difficult degradation, intensity are high, fire-retardant.
Description
Technical field
The present invention relates to engineering plastic applications more particularly to a kind of nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride and its manufactures
Method.
Background technology
Polyvinyl chloride, English abbreviation PVC is vinyl chloride monomer in initiators such as peroxide, azo-compounds；Or
The polymer being polymerized under light, heat effect by mechanism of free-radical polymerization.
Polyvinyl chloride is the white powder of impalpable structure, and the degree of branching is smaller, relative density 1.4 or so, glass transition temperature
77-90 DEG C, 170 DEG C or so start to decompose, poor to the stability of light and heat, in 100 DEG C or more or through a long time exposure in sunshine, just
It can decompose and generate hydrogen chloride, and further autocatalysis is decomposed, and causes discoloration, physical mechanical property also declines rapidly, in reality
Stabilizer is must be added to improve the stability to light and heat in the application of border, but additive of the prior art contains to nature
The poisonous and hazardous composition in boundary.
Therefore, be badly in need of on the market a kind of chemical property is stable, anti-aging property is strong, light sensitivity is low, difficult degradation, intensity are high,
Fire-retardant nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride and its manufacturing method.
The content of the invention
In view of the above defects of the prior art, the present invention is intended to provide a kind of chemical property is stable, ageing resistance
Can it is strong, light sensitivity is low, difficult degradation, intensity are high, fire-retardant nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride and its manufacturing method.
To achieve these goals, the present invention uses following technical scheme：A kind of nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride
Manufacturing method, comprise the following steps：
1) prepare before production
1. raw material prepare：Prepare enough hydrogen chloride, enough ethylene, by weight sufficient amount of oxygen, double (3,5- bis- uncles of preparation
Butyl -4- benzylphosphonic acids mono ethyl ester) 5 parts -8 parts of nickel, 5 parts -8 parts of magnesium hydroxide, 3 parts -5 parts of benzoic ether, sodium soap 3
- 5 parts of part, 3 parts -5 parts of niter cake, 5 parts of N-N ' methylene-bis-acrylamides；
2. auxiliary process material prepares：Prepare 1 part -2 parts of magnesium chloride by weight；
3. equipment and frock prepare：Prepare pressure vessel, reaction kettle；
2) modified polyvinyl chloride manufactures
1. by the stage 1) in the step benzoic ether, niter cake, N-N ' methylene-bis-acrylamides and the stage that 1. prepare
1) magnesium chloride that in 2. step prepares is uniformly mixed and is added in reaction kettle；
2. 1. reaction kettle that step is obtained is positioned in pressure vessel, led in pressure vessel with 4: 8: 3 volume ratio
Enter the stage 1) in step 1. prepare ethylene, hydrogen chloride, oxygen gas, until pressure 2.5MPa-2.8MPa in pressure vessel；
3. being warming up to 235 DEG C -240 DEG C, continue 4h-5h, recycle the miscellaneous gas of unreacted, obtain reactant, which is pre-
System material；
4. prefabricated material is heated to 190 DEG C -200 DEG C, the prefabricated material of flow-like is obtained, the stage is added in the prefabricated material of flow-like
1) double (3,5- di-tert-butyl-4-hydroxyl benzyl phosphonic acids mono ethyl ester) nickel, magnesium hydroxide, the sodium soaps that in 1. step prepares, add
1.5MPa-2.0MPa is depressed into, obtains modified polyvinyl chloride；
5. using the extrusion pressure of 35MPa-50Mpa, modified polyvinyl chloride is squeezed out and prepared after dwell time 40s-45s
Into blank to get to required nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride.
Using the above method manufacture nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride, production raw material include hydrogen chloride, ethylene,
Oxygen, double (3,5- di-tert-butyl-4-hydroxyl benzyl phosphonic acids mono ethyl ester) 5 parts -8 parts of nickel, 5 part -8 of magnesium hydroxides by weight
Part, 3 parts -5 parts of benzoic ether, 3 parts -5 parts of sodium soap, 3 parts -5 parts of niter cake, 5 parts of N-N ' methylene-bis-acrylamides.
With existing Technical comparing, the present invention has the following advantages as a result of said program：(1) with hydrogen chloride, ethylene,
Oxygen is copolymerization raw material, niter cake is antioxidant, benzoic ether is intermediate, magnesium chloride is catalyst, N-N ' methylenes
Base-bisacrylamide is crosslinking agent, double (3,5- di-tert-butyl-4-hydroxyl benzyl phosphonic acids mono ethyl ester) nickel, magnesium hydroxide are to be modified
Agent is polymerized under high temperature, high pressure, easy realization simple for process, good economy performance.(2) polyvinyl chloride with routine techniques is compared,
It is with the addition of double (3,5- di-tert-butyl-4-hydroxyl benzyl phosphonic acids mono ethyl ester) nickel and magnesium hydroxide, (3,5- bis- tertiary fourths double among these
Base -4- benzylphosphonic acids mono ethyl ester) nickel can receive the energy that micel is absorbed in plastic polyvinyl chloride, and by these energy
Amount is exhaled in the form of heat, fluorescence or phosphorescence, so as to protect polymer from the destruction of ultraviolet light；Magnesium hydroxide is one
Kind of halogen-free flame retardants, by being thermally decomposed when, are released with reference to water, substantial amounts of latent heat are absorbed, to reduce the synthesis material that it is filled
Expect the surface temperature in flame, play an important role of that inhibiting polymer decomposes and generated fuel gas is cooled down.(3)
Under the action of N-N ' methylene-bis-acrylamide crosslinking agents, polyvinyl chloride of the invention reticulates knot from the crosslinking of chain assembling structure
Structure, stability are greatly improved, and under sunshine in use, under the action of ultraviolet light, the slow crosslinking in later stage is still being sent out
It is raw, the present invention is made increasingly to stablize in use, since net structure is highly stable structure, and without stress concentration
Direction and notch sensitivity, therefore the present invention has that (tearing strength is about compared to the higher intensity of routine techniques and tear resistance
95MPa or so, routine techniques 60MPa).
Specific embodiment
Embodiment 1：
A kind of nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride, production raw material include hydrogen chloride, ethylene, oxygen, by weight
Double (3,5- di-tert-butyl-4-hydroxyl benzyl phosphonic acids mono ethyl ester) nickel 5Kg, magnesium hydroxide 5Kg, benzoic ether 3Kg, the aliphatic acid of meter
Sodium 3Kg, niter cake 3Kg, N-N ' methylene-bis-acrylamides 5Kg.
The manufacturing method of above-mentioned nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride, comprises the following steps：
1) prepare before production
1. raw material prepare：Prepare enough hydrogen chloride, enough ethylene, by weight sufficient amount of oxygen, double (3,5- bis- uncles of preparation
Butyl -4- benzylphosphonic acids mono ethyl ester) nickel 5Kg, magnesium hydroxide 5Kg, benzoic ether 3Kg, sodium soap 3Kg, niter cake
3Kg, N-N ' methylene-bis-acrylamide 5Kg；
2. auxiliary process material prepares：Prepare magnesium chloride 1Kg by weight；
3. equipment and frock prepare：Prepare pressure vessel, reaction kettle；
2) modified polyvinyl chloride manufactures
1. by the stage 1) in the step benzoic ether, niter cake, N-N ' methylene-bis-acrylamides and the stage that 1. prepare
1) magnesium chloride that in 2. step prepares is uniformly mixed and is added in reaction kettle；
2. 1. reaction kettle that step is obtained is positioned in pressure vessel, led in pressure vessel with 4: 8: 3 volume ratio
Enter the stage 1) in step 1. prepare ethylene, hydrogen chloride, oxygen gas, until pressure 2.5MPa in pressure vessel；
3. being warming up to 235 DEG C, continue 4h, recycle the miscellaneous gas of unreacted, obtain reactant, which is prefabricated material；
4. prefabricated material is heated to 190 DEG C, obtain the prefabricated material of flow-like, the stage 1 added in the prefabricated material of flow-like) in step
Rapid double (3,5- di-tert-butyl-4-hydroxyl benzyl phosphonic acids mono ethyl ester) nickel, magnesium hydroxide, the sodium soaps 1. prepared, are forced into
1.5MPa obtains modified polyvinyl chloride；
5. using the extrusion pressure of 35MPa, modified polyvinyl chloride is squeezed out after dwell time 40s and is prepared into blank, i.e.,
Nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride needed for obtaining.
Embodiment 2：
It is whole consistent with embodiment 1, it is in place of difference：
A kind of nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride, production raw material include hydrogen chloride, ethylene, oxygen, by weight
Double (3,5- di-tert-butyl-4-hydroxyl benzyl phosphonic acids mono ethyl ester) nickel 8Kg, magnesium hydroxide 8Kg, benzoic ether 5Kg, the aliphatic acid of meter
Sodium 5Kg, niter cake 5Kg, N-N ' methylene-bis-acrylamides 5Kg.
The manufacturing method of above-mentioned nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride, comprises the following steps：
1) prepare before production
1. raw material prepare：Prepare enough hydrogen chloride, enough ethylene, by weight sufficient amount of oxygen, double (3,5- bis- uncles of preparation
Butyl -4- benzylphosphonic acids mono ethyl ester) nickel 8Kg, magnesium hydroxide 8Kg, benzoic ether 5Kg, sodium soap 5Kg, niter cake
5Kg, N-N ' methylene-bis-acrylamide 5Kg；
2. auxiliary process material prepares：Prepare magnesium chloride 2Kg by weight；
2) modified polyvinyl chloride manufactures
2. 1. reaction kettle that step is obtained is positioned in pressure vessel, led in pressure vessel with 4: 8: 3 volume ratio
Enter the stage 1) in step 1. prepare ethylene, hydrogen chloride, oxygen gas, until pressure 2.8MPa in pressure vessel；
3. being warming up to 240 DEG C, continue 5h, recycle the miscellaneous gas of unreacted, obtain reactant, which is prefabricated material；
4. prefabricated material is heated to 200 DEG C, obtain the prefabricated material of flow-like, the stage 1 added in the prefabricated material of flow-like) in step
Rapid double (3,5- di-tert-butyl-4-hydroxyl benzyl phosphonic acids mono ethyl ester) nickel, magnesium hydroxide, the sodium soaps 1. prepared, are forced into
2.0MPa obtains modified polyvinyl chloride；
5. using the extrusion pressure of 5OMpa, modified polyvinyl chloride is squeezed out after dwell time 45s and is prepared into blank, i.e.,
Nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride needed for obtaining.
The foregoing description of the disclosed embodiments, only for professional and technical personnel in the field is enable to realize or use this
Invention.A variety of modifications of these embodiments will be apparent for those skilled in the art, institute herein
The General Principle of definition can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore,
The present invention is not intended to be limited to the embodiments shown herein, and is to fit to special with principles disclosed herein and novelty
The consistent most wide scope of point.
Claims (2)
1. a kind of manufacturing method of nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride, it is characterised in that comprise the following steps：
1) prepare before production
1. raw material prepare：Prepare enough hydrogen chloride, enough ethylene, by weight sufficient amount of oxygen, double (3, the 5- bis- tertiary fourths of preparation
Base -4- benzylphosphonic acids mono ethyl ester) 5 parts -8 parts of nickel, 5 parts -8 parts of magnesium hydroxide, 3 parts -5 parts of benzoic ether, sodium soap 3
- 5 parts of part, 3 parts -5 parts of niter cake, 5 parts of N-N ' methylene-bis-acrylamides；
2. auxiliary process material prepares：Prepare 1 part -2 parts of magnesium chloride by weight；
3. equipment and frock prepare：Prepare pressure vessel, reaction kettle；
2) modified polyvinyl chloride manufactures
1. by the stage 1) in the step benzoic ether, niter cake, N-N ' methylene-bis-acrylamides and the stage 1 that 1. prepare) in
2. magnesium chloride that step prepares is uniformly mixed and is added in reaction kettle；
2. 1. reaction kettle that step is obtained is positioned in pressure vessel, rank is passed through with 4: 8: 3 volume ratio in pressure vessel
Section 1) in step 1. prepare ethylene, hydrogen chloride, oxygen gas, until pressure 2.5MPa-2.8MPa in pressure vessel；
3. being warming up to 235 DEG C -240 DEG C, continue 4h-5h, recycle the miscellaneous gas of unreacted, obtain reactant, which is prefabricated material；
4. prefabricated material is heated to 190 DEG C -200 DEG C, the prefabricated material of flow-like is obtained, the stage 1 is added in the prefabricated material of flow-like) in
1. double (3,5- di-tert-butyl-4-hydroxyl benzyl phosphonic acids mono ethyl ester) nickel, magnesium hydroxide, sodium soaps that step prepares, are forced into
1.5MPa-2.0MPa obtains modified polyvinyl chloride；
5. using the extrusion pressure of 35MPa-50Mpa, modified polyvinyl chloride is squeezed out after dwell time 40s-45s and is prepared into base
Material is to get to required nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride.
2. a kind of nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride manufactured using claim 1 the method, it is characterised in that：This is poly-
Vinyl chloride production raw material include hydrogen chloride, ethylene, oxygen, double (3,5- di-tert-butyl-4-hydroxyl benzyl phosphines by weight
Sour mono ethyl ester) 5 parts -8 parts of nickel, 5 parts -8 parts of magnesium hydroxide, 3 parts -5 parts of benzoic ether, 3 parts -5 parts of sodium soap, niter cake 3
Part -5 parts, 5 parts of N-N ' methylene-bis-acrylamides.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711498059.8A CN108084318A (en) | 2017-12-28 | 2017-12-28 | A kind of nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride and its manufacturing method |
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| CN201711498059.8A CN108084318A (en) | 2017-12-28 | 2017-12-28 | A kind of nuisanceless flame-resistant high-temperature-resistant polyvinyl chloride and its manufacturing method |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1077963A (en) * | 1992-04-29 | 1993-11-03 | Basf公司 | Aqueous polymer dispersion |
| CN104448092A (en) * | 2014-12-29 | 2015-03-25 | 周大胜 | Impact-resistant chloroethylene copolymer resin and preparation method thereof |
| CN104558428A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | High-toughened chloroethylene grafted copolymer and preparation method thereof |
| CN105968272A (en) * | 2016-06-28 | 2016-09-28 | 杭州电化集团有限公司 | Preparation method of extinction polyvinyl chloride resin |
-
2017
- 2017-12-28 CN CN201711498059.8A patent/CN108084318A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1077963A (en) * | 1992-04-29 | 1993-11-03 | Basf公司 | Aqueous polymer dispersion |
| CN104558428A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | High-toughened chloroethylene grafted copolymer and preparation method thereof |
| CN104448092A (en) * | 2014-12-29 | 2015-03-25 | 周大胜 | Impact-resistant chloroethylene copolymer resin and preparation method thereof |
| CN105859943A (en) * | 2014-12-29 | 2016-08-17 | 周大胜 | Preparation method of shock-resistant vinyl chloride copolymer resin |
| CN105968272A (en) * | 2016-06-28 | 2016-09-28 | 杭州电化集团有限公司 | Preparation method of extinction polyvinyl chloride resin |
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Application publication date: 20180529 |