CN109265587A - A kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminates agent emulsion and preparation method thereof - Google Patents
A kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminates agent emulsion and preparation method thereof Download PDFInfo
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- CN109265587A CN109265587A CN201811053881.8A CN201811053881A CN109265587A CN 109265587 A CN109265587 A CN 109265587A CN 201811053881 A CN201811053881 A CN 201811053881A CN 109265587 A CN109265587 A CN 109265587A
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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
- C08F14/00—Homopolymers and 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
- C08F14/02—Monomers containing chlorine
- C08F14/04—Monomers containing two carbon atoms
- C08F14/06—Vinyl chloride
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Abstract
The present invention provides a kind of anti-freeze type high fever ageing whiteness polyvinyl chloride and terminates agent emulsion and preparation method thereof, is related to a kind of technical field of fine.The invention is prepared by the raw material comprising following weight parts: 10-15 parts of bisphenol-A, 7-10 parts of acetone semicarbazone thiocarbamide, 8-10 parts of phosphite ester heat stabilizer, 12-16 parts of block polyether emulsifier of aliphatic epoxy ethane epoxy propane, 1-3 parts of dispersion stabilizer, 10-15 parts of antifreezing agent.The present invention improves the heat ageing whiteness of terminator, and the anti-freeze type polyvinyl chloride for producing stable system terminates agent emulsion.
Description
Technical field
The present invention relates to a kind of technical field of fine, are applied to Polymer Synthesizing auxiliary industry and Corvic
Production industry terminates agent emulsion and preparation method thereof more particularly to a kind of anti-freeze type high fever ageing whiteness polyvinyl chloride.
Background technique
Having the call with terminator during polyvinyl chloride resin production, wherein it is most to terminate agent emulsion dosage,
Account for about the 85% of domestic terminator consumption.
1, terminating agent emulsion is later period eighties domestic PVC auxiliary industry according to domestic market demand self-developing
A kind of low cost aqueous termination agent emulsion, since the auxiliary agent is water-based emulsion, auxiliary agent is easy to use, is not required to prepare, can be fast
Speed is dissolved in polymerization system, and termination effect is good, production of resins cost is reduced, by the joyous of polyvinyl chloride resin production producer
It meets.
But with the high speed development of China's PVC Industry, also the heat ageing whiteness of Corvic is proposed
In Corvic national standard there is the New Set of resin heat ageing whiteness in new requirement, it is desirable that the resin heat of detection
Ageing whiteness reaches 78 or more.Moreover, some resin processing plants are due to producing high whiteness resin, it is also desirable to which resin heat ageing whiteness reaches
80-90.Although the control of polymerization temperature during resin heat ageing whiteness and polyvinyl chloride resin production, resin initial coloration,
The water content and acetylene content of vinyl chloride monomer suffer from indivisible connection, are also the domestic section for terminating agent emulsion still
It grinds and production is put forward new requirements.
2, since terminator is water-based emulsion, the packaging used is mostly 200kg plastic barrel or metal bucket packaging, is easy in winter
Freeze, dissolve it is extremely difficult, before auxiliary agent, it is necessary to could be used after in advance dissolving the workshop that charging basket is put into heating.
In the southern area of not heating, it is necessary to charging basket is put into Special baking room, draw to workshop and use again after auxiliary agent is dissolved.It solves
The antifreeze problem of auxiliary agent becomes a big problem of terminator production.Past is antifreeze to solve the problems, such as, has producer terminating agent emulsion
In antifreezing agent is added, still, terminate agent emulsion severe delamination, cannot use.
3, terminating agent emulsion production is not no byproduct, but every production kettle termination agent emulsion will brush a kettle,
It is exactly that reaction kettle is added in tap water and detergent, starts stirring and carry out washing kettle, then again bleed off washing water, makes again certainly
Water starts stirring and washes kettle twice, finally kettle washing water is bled off again, just can be carried out next kettle production, not only waste is a large amount of
Water source, and kettle washing water contains toxic bisphenol-A terminator, pollutes the environment.
Summary of the invention
Aiming at the shortcomings existing in the above problems, the present invention provides a kind of anti-freeze type high fever ageing whiteness polyvinyl chloride
Agent emulsion and preparation method thereof is terminated, the heat ageing whiteness which raises terminator is made, the anti-freeze type for producing stable system is poly-
Vinyl chloride terminates agent emulsion.
To solve the above-mentioned problems, the present invention provides a kind of anti-freeze type high fever ageing whiteness polyvinyl chloride termination agent emulsion,
Wherein, it is prepared by the raw material comprising following weight parts: 10-15 parts of bisphenol-A, 7-10 parts of acetone semicarbazone thiocarbamide terminator,
8-10 parts of phosphite ester heat stabilizer, 12-16 parts of block polyether emulsifier of aliphatic epoxy ethane epoxy propane, dispersion stabilizer 1-
3 parts, 10-15 parts of antifreezing agent.
Preferably, it is prepared by the raw material comprising following weight parts: 10 parts of bisphenol-A, acetone semicarbazone thiocarbamide terminator 7
Part, 8 parts of phosphite ester heat stabilizer, 12 parts of emulsifier of aliphatic epoxy ethane epoxy propane block polyether, 1 part of dispersion stabilizer,
10 parts of antifreezing agent.
Preferably, be prepared by the raw material comprising following weight parts: 12.5 parts of bisphenol-A, acetone semicarbazone thiocarbamide is made eventually
Only 8.5 parts of agent, 9 parts of phosphite ester heat stabilizer, 14 parts of emulsifier of aliphatic epoxy ethane epoxy propane block polyether, stably dispersing
2 parts of agent, 13 parts of antifreezing agent.
Preferably, be prepared by the raw material comprising following weight parts: 15 parts of bisphenol-A, acetone semicarbazone thiocarbamide terminates
10 parts of agent, 10 parts of phosphite ester heat stabilizer, 16 parts of emulsifier of aliphatic epoxy ethane epoxy propane block polyether, dispersion stabilizer
3 parts, 15 parts of antifreezing agent.
Preferably, dispersion stabilizer uses polyvinyl alcohol, can preferably control the stabilization for terminating agent emulsion.
Preferably, antifreezing agent uses methanol or ethyl alcohol.
A kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminates the preparation method of agent emulsion, wherein the following steps are included:
S10, it checks that polymeric kettle safe condition is good, deionized water and poly-vinyl alcohol solution is added from charging spout by formula
In kettle；
S20, kettle cover is opened, phosphite ester heat stabilizer is added, terminator bisphenol-A and acetone semicarbazone thiocarbamide is added, adds
Enter aliphatic epoxy ethane epoxy propane block polyether nonionic emulsifier, is then shut off polymeric kettle feed opening；
S30, stirring is started, material in kettle is raised to 70 DEG C, insulated and stirred 120 minutes；
S40, polymeric kettle cooling water inlet valve is opened, material temperature in kettle is dropped to 40 DEG C or less；
S50, poly-vinyl alcohol solution is added, antifreezing agent is added and stirs evenly, the lotion produced is ground with colloid mill, it is raw
Output finished product terminates agent emulsion.
Compared with prior art, the invention has the following advantages that
1, improve the heat ageing whiteness of terminator: according to the termination mechanism of suspension polymerization of VC, we are to terminator
Ingredient carried out new design, reduce production cost 30% and also use high-temperature thermal stability other than having used fast terminator
Agent, the material are cooperateed with terminator, so that the heat ageing whiteness for terminating agent emulsion is significantly improved, are shown experimentally that, such as
Fruit vinyl chloride monomer water content and acetylene content are qualified, are controlled using computer programs, terminate agent emulsion using the present invention
The resin heat ageing whiteness of production is up to 80-95.
2, the anti-freeze type polyvinyl chloride for producing stable system terminates agent emulsion: terminating agent emulsion by using new emulsification
Terminator is effectively guaranteed using aliphatic epoxy ethane epoxy propane block polyether nonionic emulsifier system in agent system
Stabilization of the lotion after refrigerant is added, lotion do not freeze after -20 DEG C of freezings, and not stratified, good fluidity solves more
The antifreeze problem for the termination agent emulsion not solved in year, simplifies operating process, improves product quality, makes to terminate agent emulsion more
It is easy to use.Moreover, the present invention can be according to user demand, the termination agent emulsion for producing different antifreeze temperature is used for everybody.
3, kettle is washed using high pressure de-ionized water, the kettle washing water of recycling can use as process water in next batch, prevent
Terminator production is discharged pollutes caused by toxic kettle washing water: due to using high-pressure washing kettle, can also will gather without using detergent
Kettle is closed to clean up.Kettle, such as a 3m are washed using old technology3Polymeric kettle need to use water 9m3, this process water consumption is old work
The 1/120 of skill, only 0.75m3.Due to making that kettle is washed with deionized water, the kettle washing water of recycling can the conduct in next batch production
Process water uses, and is truly realized none drop discharge of wastewater.Pollution caused by kettle washing water is not only prevented, and reduces public work
Journey consumption.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, the present invention is made below with reference to example
It is further described, but example is not as a limitation of the invention.
Embodiment 1
A kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminate agent emulsion by the raw material preparation comprising following weight parts and
At: 10 parts of bisphenol-A, 7 parts of acetone semicarbazone thiocarbamide terminator, 8 parts of phosphite ester heat stabilizer, aliphatic epoxy ethane epoxy propane
12 parts of block polyether emulsifier, 1 part of polyvinyl alcohol dispersion stabilizer, 10 parts of methanol antifreezing agent.
Dispersion stabilizer uses polyvinyl alcohol, can preferably control the stabilization for terminating agent emulsion.
Antifreezing agent uses methanol.
A kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminates the preparation method of agent emulsion, wherein the following steps are included:
S10, it checks that polymeric kettle safe condition is good, deionized water and poly-vinyl alcohol solution is added from charging spout by formula
In kettle；
S20, kettle cover is opened, phosphite ester heat stabilizer is added, terminator bisphenol-A and acetone semicarbazone thiocarbamide is added, adds
Enter aliphatic epoxy ethane epoxy propane block polyether nonionic emulsifier, is then shut off polymeric kettle feed opening；
S30, stirring is started, material in kettle is raised to 70 DEG C, insulated and stirred 120 minutes；
S40, polymeric kettle cooling water inlet valve is opened, material temperature in kettle is dropped to 40 DEG C or less；
S50, addition antifreezing agent stir evenly, and the lotion produced is ground with colloid mill, produce finished product terminator cream
Liquid.
The terminator for using the formula system of embodiment 1 to prepare is white emulsion, PH6-8, non-volatile phenol content >=36%,
Specific gravity (20 DEG C, g/ml) >=0.9, -20 DEG C freezing test 72 hours, material does not freeze, emulsion-stabilizing, good fluidity.It is long
Phase storage test stationary phase >=12 month.It is used in Production of PVC, heat ageing whiteness is between 80-95, technical indicator
More than this company standard, it is better than industry universal terminator standard.
Embodiment 2
A kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminate agent emulsion by the raw material preparation comprising following weight parts and
At: 12.5 parts of bisphenol-A, acetone semicarbazone thiocarbamide makees 8.5 parts of terminator, and 9 parts of phosphite ester heat stabilizer, aliphatic epoxy ethane ring
14 parts of Ethylene Oxide block polyether emulsifier, 2 parts of polyvinyl alcohol dispersion stabilizer, 13 parts of methanol antifreezing agent.
Dispersion stabilizer uses polyvinyl alcohol, can preferably control the stabilization for terminating agent emulsion.
Antifreezing agent uses methanol.
A kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminates the preparation method of agent emulsion, comprising the following steps:
S10, it checks that polymeric kettle safe condition is good, adds deionized water and poly-vinyl alcohol solution from charging spout by formula
Enter in kettle,；
S20, kettle cover is opened, terminator bisphenol-A and acetone semicarbazone thiocarbamide is added, phosphite ester heat stabilizer is added, adds
Enter aliphatic epoxy ethane epoxy propane block polyether nonionic emulsifier, is then shut off polymeric kettle feed opening；
S30, stirring is started, material in kettle is raised to 70 DEG C, insulated and stirred 120 minutes；
S40, polymeric kettle cooling water inlet valve is opened, material temperature in kettle is dropped to 40 DEG C or less；
S50, addition antifreezing agent stir evenly, and the lotion produced is ground with colloid mill, produce finished product terminator cream
Liquid.
The terminator for using the formula system of embodiment 2 to prepare is white emulsion, PH6-8, non-volatile phenol content >=36%,
Specific gravity (20 DEG C, g/ml) >=0.9, -20 DEG C freezing test 72 hours, material does not freeze, emulsion-stabilizing, good fluidity.It is long
Phase storage test stationary phase >=12 month.It is used in Production of PVC, heat ageing whiteness is between 80-95, technical indicator
More than this company standard, it is better than industry universal terminator standard.
Embodiment 3
A kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminate agent emulsion by the raw material preparation comprising following weight parts and
At: 15 parts of bisphenol-A, acetone semicarbazone thiocarbamide makees 10 parts of terminator, and 10 parts of phosphite ester heat stabilizer, aliphatic epoxy ethane epoxy
16 parts of propane block polyether emulsifier, 3 parts of polyvinyl alcohol dispersion stabilizer, 15 parts of methanol antifreezing agent.
Dispersion stabilizer uses polyvinyl alcohol, can preferably control the stabilization for terminating agent emulsion.
Antifreezing agent uses methanol.
A kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminates agent emulsion and preparation method thereof, wherein including following step
It is rapid:
S10, it checks that polymeric kettle safe condition is good, deionized water and poly-vinyl alcohol solution is added from charging spout by formula
In kettle；
S20, kettle cover is opened, phosphite ester heat stabilizer is added, terminator bisphenol-A and acetone semicarbazone thiocarbamide is added, adds
Enter aliphatic epoxy ethane epoxy propane block polyether nonionic emulsifier, is then shut off polymeric kettle feed opening；
S30, stirring is started, material in kettle is raised to 70 DEG C, insulated and stirred 120 minutes；
S40, polymeric kettle cooling water inlet valve is opened, material temperature in kettle is dropped to 40 DEG C or less；
S50, addition antifreezing agent stir evenly, and the lotion produced is ground with colloid mill, produce finished product terminator cream
Liquid.
The terminator for using the formula system of embodiment 3 to prepare is white emulsion, PH6-8, non-volatile phenol content >=36%,
Specific gravity (20 DEG C, g/ml) >=0.9, -20 DEG C freezing test 72 hours, material does not freeze, emulsion-stabilizing, good fluidity.It is long
Phase storage test stationary phase >=12 month.It is used in Production of PVC, heat ageing whiteness is between 80-95, technical indicator
More than this company standard, it is better than industry universal terminator standard.
In the present embodiment, is studied for agent emulsion composition principle is terminated, new synthesis mechanism is established, to termination
The component of agent has carried out new design, reduces the production cost 30% of terminator, increases the dosage of Quick stop agent, improves
The termination speed of terminator increases new heat stabilizer to improve resin heat ageing whiteness, such as phosphite ester etc. is used
Amount is 10-15 parts.
In the present embodiment, agent emulsion is terminated in order to produce anti-freeze type, prevents creaming of emulsion, dispersion of the present invention to lotion
Agent, emulsifier, antifreeze systems have carried out a large amount of test, have selected cost performance high, with strong points, efficient New-type adjuvant,
Terminator synthesizing formula is improved, nonionic emulsifier such as aliphatic epoxy ethane epoxy propane block polyether is used
System, produces stable anti-freeze type PVC and terminates agent emulsion, lotion is not stratified at -20 DEG C, there is good stream by 12-16 parts of dosage
Dynamic property, stationary phase are more than old technology 6 months levels, and the present invention terminates agent emulsion placement 12 months or more still with good
Stability.
In the present embodiment, according to the composition principle of terminator, using charging process, process water is first added in kettle, is prevented
Only a large amount of oiliness materials adhere on kettle wall, after production finishes, using high pressure water washing cart rinse polymeric kettle inner wall, stirring and
Ancillary equipment surface, it is easy to wash down material in kettle.Water due to rinsing polymeric kettle uses deionized water, washes the water of kettle
It is recovered in plastic barrel by bottom valve, is added in kettle and uses as process water in production next time, thoroughly prevented to wash kettle and given up
The discharge of water is accomplished without a drop waste water.
High fever ageing whiteness polyvinyl chloride of the present invention terminates agent emulsion compared with the technical indicator of old technology termination agent emulsion:
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (7)
1. a kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminates agent emulsion, which is characterized in that by including following weight parts
Raw material is prepared: 10-15 parts of bisphenol-A, 7-10 parts of acetone semicarbazone thiocarbamide, and 8-10 parts of phosphite ester heat stabilizer, aliphatic ring
Oxidative ethane propylene oxide block polyethers emulsifies 12-16 parts, 1-3 parts of dispersion stabilizer, 10-15 parts of antifreezing agent.
2. anti-freeze type high fever ageing whiteness polyvinyl chloride as described in claim 1 terminates agent emulsion, which is characterized in that by comprising
The raw material of following weight parts is prepared: 10 parts of bisphenol-A, acetone semicarbazone thiocarbamide makees 7 parts of terminator, phosphite ester heat stabilizer
7 parts, 12 parts of emulsifier, 1 part of dispersion stabilizer, 10 parts of antifreezing agent of aliphatic epoxy ethane epoxy propane block polyether.
3. anti-freeze type high fever ageing whiteness polyvinyl chloride as described in claim 1 terminates agent emulsion, which is characterized in that by comprising
The raw material of following weight parts is prepared: 12.5 parts of bisphenol-A, acetone semicarbazone thiocarbamide makees 8.5 parts of terminator, and phosphite ester heat is steady
Determine 9 parts of agent, 14 parts of emulsifier, 2 parts of dispersion stabilizer, 13 parts of antifreezing agent of aliphatic epoxy ethane epoxy propane block polyether.
4. anti-freeze type high fever ageing whiteness polyvinyl chloride as described in claim 1 terminates agent emulsion, which is characterized in that by comprising
The raw material of following weight parts is prepared: 15 parts of bis-phenol, acetone semicarbazone thiocarbamide makees 10 parts of terminator, phosphite ester heat stabilizer
10 parts, 16 parts of emulsifier, 3 parts of dispersion stabilizer, 15 parts of antifreezing agent of aliphatic epoxy ethane epoxy propane block polyether.
5. anti-freeze type high fever ageing whiteness polyvinyl chloride as described in claim 1 terminates agent emulsion, which is characterized in that dispersion is steady
Agent is determined using polyvinyl alcohol, can preferably control the stabilization for terminating agent emulsion.
6. anti-freeze type high fever ageing whiteness polyvinyl chloride as described in claim 1 terminates agent emulsion, which is characterized in that antifreezing agent
Use methanol or ethyl alcohol.
7. a kind of anti-freeze type high fever ageing whiteness polyvinyl chloride as described in claim 1 terminates the preparation method of agent emulsion,
It is characterized in that, comprising the following steps:
S10, it checks that polymeric kettle safe condition is good, deionized water and polyvinyl alcohol is added in kettle from charging spout by formula；
S20, kettle cover is opened, phosphite ester heat stabilizer is added；Terminator bisphenol-A and acetone semicarbazone thiocarbamide is added, rouge is added
Race's ethylene oxide propylene oxide block polyether nonionic emulsifier, is then shut off polymeric kettle feed opening；
S30, stirring is started, material in kettle is raised to 70 DEG C, insulated and stirred 120 minutes；
S40, polymeric kettle cooling water inlet valve is opened, material temperature in kettle is dropped to 40 DEG C or less；
S50, methyl styrene is added, antifreezing agent is added and stirs evenly, the lotion produced is ground with colloid mill, is produced into
Product terminate agent emulsion.
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|---|---|---|---|
| CN201811053881.8A CN109265587A (en) | 2018-09-11 | 2018-09-11 | A kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminates agent emulsion and preparation method thereof |
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| CN201811053881.8A CN109265587A (en) | 2018-09-11 | 2018-09-11 | A kind of anti-freeze type high fever ageing whiteness polyvinyl chloride terminates agent emulsion and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0069702A2 (en) * | 1981-07-06 | 1983-01-12 | Ciba-Geigy Ag | Stop chain agent for vinylchloride polymerisation |
| CN102432715A (en) * | 2011-11-28 | 2012-05-02 | 河北盛华化工有限公司 | Preparation method of emulsion-type termination agent special for polymerization of polyvinyl chloride (PVC) |
| CN108424480A (en) * | 2018-03-28 | 2018-08-21 | 鄂尔多斯市瀚博科技有限公司 | A kind of efficient terminator of polyvinyl chloride polymerization and its application |
-
2018
- 2018-09-11 CN CN201811053881.8A patent/CN109265587A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0069702A2 (en) * | 1981-07-06 | 1983-01-12 | Ciba-Geigy Ag | Stop chain agent for vinylchloride polymerisation |
| CN102432715A (en) * | 2011-11-28 | 2012-05-02 | 河北盛华化工有限公司 | Preparation method of emulsion-type termination agent special for polymerization of polyvinyl chloride (PVC) |
| CN108424480A (en) * | 2018-03-28 | 2018-08-21 | 鄂尔多斯市瀚博科技有限公司 | A kind of efficient terminator of polyvinyl chloride polymerization and its application |
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Application publication date: 20190125 |