CN106750246A - A kind of frost resistance emulsifying agent and its production technology - Google Patents
A kind of frost resistance emulsifying agent and its production technology Download PDFInfo
- Publication number
- CN106750246A CN106750246A CN201611234098.2A CN201611234098A CN106750246A CN 106750246 A CN106750246 A CN 106750246A CN 201611234098 A CN201611234098 A CN 201611234098A CN 106750246 A CN106750246 A CN 106750246A
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- Prior art keywords
- catalyst
- oxirane
- emulsifying agent
- fatty alcohols
- reactor
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2642—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds characterised by the catalyst used
- C08G65/2645—Metals or compounds thereof, e.g. salts
- C08G65/2648—Alkali metals or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2642—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds characterised by the catalyst used
- C08G65/2645—Metals or compounds thereof, e.g. salts
- C08G65/2651—Alkaline earth metals or compounds thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K23/00—Use of substances as emulsifying, wetting, dispersing, or foam-producing agents
Abstract
The present invention discloses a kind of frost resistance emulsifying agent, its reaction supplementary material includes the fatty alcohols 58.0%~67.0% of C12 14, alkaline mixed catalyst 0.5%~1.2%, oxirane 33.0%~42.0%, the alkaline mixed catalyst include base catalyst and alkaline earth catalyst.Its production technology is：120 DEG C~140 DEG C are heated to after first the fatty alcohols of C12 14 are mixed with alkaline mixed catalyst, vacuum dehydration, 90 DEG C of rear substitution nitrogen is then cooled to after the completion of dehydration three times, oxirane is slowly added into reactor and is reacted with the fatty alcohols of C12 14, control temperature is between 90 100 DEG C, after oxirane addition reaches technological requirement, close oxirane valve, wait to continue to react a period of time, pressure and temperature no longer fluctuates and is cooled to 70 DEG C in reactor, treatment is de-gassed to material in reactor again, degassing process time lengthening was to 1 hour.By reselecting catalyst and changing production technology, so as to reduce the congealing point and penetrating odor of fatty alcohol emulsifying agent.
Description
Technical field
The present invention is belonging to the process modification of surfactant, particularly a kind of frost resistance emulsifying agent and its production technology.
Background technology
Emulsifying agent is a kind of important industrial chemicals, and fatty alcohol series emulsifying agent is one kind of wherein large usage quantity, is accounted for
To 40% or so of the total consumption of emulsifying agent.The existing fatty alcohol series emulsifying agent mode of production mainly has two kinds, and one kind is to use
Base catalyst potassium hydroxide, its shortcoming is mainly reflected in molecular weight of product and is distributed relatively wide, easy jelly；Another kind is using acidity
Catalyst, its shortcoming is mainly reflected in irritant smell, and accessory substance is more.And existing fatty alcohol series emulsifying agent production work
Skill temperature is 130-140 DEG C, causes organic matter to produce more accessory substance during the course of the reaction, and reaction terminates rear degassing time
It is half an hour, causes the irritant smell of product；With the requirement of development and safety and the environmental protection of the modernization of industry, client is to breast
The all requirements of agent are also improved therewith, we only have improvement each side technical indicator could meet customer requirement.
The content of the invention
The object of the invention be directed to it is above-mentioned present in problem, propose a kind of frost resistance emulsifying agent and its production technology, make
Obtain the emulsifying agent and have the advantage that congealing point is low and has no irritating odor concurrently.
In order to solve the deficiency of above-mentioned technology, the technical scheme is that：A kind of frost resistance emulsifying agent, its reaction is former auxiliary
Material includes：C12-14 fatty alcohols, alkaline mixed catalyst, oxirane；On the basis of the weight of product：C12-14 fatty alcohols
58.0%~67.0%, alkaline mixed catalyst 0.5%~1.2%, oxirane 33.0%~42.0%, the alkalescence mixing
Catalyst includes base catalyst and alkaline earth catalyst.
Preferably, the base catalyst in the alkaline mixed catalyst is KOH, alkaline earth catalyst is Ba (OH)2, its
Middle KOH and Ba (OH)2Ratio be 1:1~3.
Alkaline earth catalyst Ba (OH) used in its neutral and alkali mixed catalyst2Reaction speed is slow, and the product for obtaining point
Son amount distribution is narrow, and anti-freezing property is high, after mix with base catalyst KOH, neutralized original base catalyst it is caused
Molecular weight of product distribution is relatively wide, the deficiency easily frozen, the molecular weight of product point obtained using the mixed catalyst of suitable ratio
Cloth is suitable, and anti-freezing property is high.
Another technical scheme of the invention is：A kind of production technology of frost resistance emulsifying agent, comprises the following steps：First will
C12-14 fatty alcohols are heated to 120 DEG C~140 DEG C after mixing with alkaline mixed catalyst, and vacuum dehydration is then dropped after the completion of dehydration
Be slowly added into reactor oxirane and the reaction of C12-14 fatty alcohols, control temperature to 90 DEG C of rear substitution nitrogen three times by temperature
Degree after oxirane addition reaches technological requirement, closes oxirane valve between 90-100 DEG C, waits to continue to react one section
Time, pressure and temperature no longer fluctuates and is cooled to 70 DEG C in reactor, then is de-gassed treatment to material in reactor, at degassing
Reason time lengthening was to 1 hour.
Original acidulous catalyst is changed to alkalescence mixed by above-mentioned production technology using the fatty alcohol of natural carbochain 12-14
Close catalyst, alkaline earth catalyst Ba (OH) used in its neutral and alkali mixed catalyst2Reaction speed is slow, and the product for obtaining point
Son amount distribution is narrow, and anti-freezing property is high, after mix with base catalyst KOH, neutralized original base catalyst it is caused
Molecular weight of product distribution is relatively wide, the deficiency easily frozen, the molecular weight of product point obtained using the mixed catalyst of suitable ratio
Cloth is suitable, and anti-freezing property is high；In addition low-temp reaction, reaction temperature are controlled during ethoxylation：90-100 DEG C, reaction terminates
Proper extension degassing time was to 1 hour afterwards, so that low-boiling by-products and penetrating odor in product are reduced, it is final to cause fat
Alcohol emulsifying agent congealing point is than 10 DEG C or so of common fats alcohol emulsifying agent reduction；Smell is also similar with mill run without excitant, produces
Product quality has greatly improved, so as to also ensure that the quality requirement of downstream product.
The advantage of above-mentioned freeze proof emulsifying agent is as follows：1st, it is small to reactor corrosivity using base catalyst, while low temperature is anti-
Should cause that reaction is more steady, reduce the generation of accessory substance；2nd, have no irritating odor and low congealing point also complies with development of modern industry
Need, have no irritating odor guarantee safety of workers while, be more beneficial for being promoted aborning, low congealing point also cause its
Under conditions of southern winter and northern low temperature, enterprise is facilitated to produce and get the nod.
Specific embodiment
The centrifugal device to the embodiment of the present invention is described in further detail below：
The present invention is a kind of frost resistance emulsifying agent, and its reaction supplementary material includes：C12-14 fatty alcohols, alkaline mixed catalytic
Agent, oxirane；On the basis of the weight of product：C12-14 fatty alcohols 58.0%~67.0%, alkaline mixed catalyst 0.5%
~1.2%, oxirane 33.0%~42.0%, the base catalyst in the alkaline mixed catalyst is KOH, alkaline earth catalysis
Agent is Ba (OH)2, wherein KOH and Ba (OH)2Ratio be 1:1.
The production technology of above-mentioned frost resistance emulsifying agent, comprises the following steps：First C12-14 fatty alcohols are mixed with alkalescence and is urged
130 DEG C are heated to after agent mixing, vacuum dehydration is then cooled to 90 DEG C of rear substitution nitrogen three times after the completion of dehydration, by epoxy second
Alkane reacts in being slowly added into reactor with C12-14 fatty alcohols, and between 95 DEG C, oxirane addition reaches control temperature
After technological requirement, oxirane valve is closed, wait to continue to react a period of time, pressure and temperature no longer fluctuates cooling in reactor
To 70 DEG C, then treatment is de-gassed to material in reactor, degassing process time lengthening was to 1 hour.
Original acidulous catalyst is changed to alkalescence mixed by above-mentioned production technology using the fatty alcohol of natural carbochain 12-14
Close catalyst, alkaline earth catalyst Ba (OH) used in its neutral and alkali mixed catalyst2Reaction speed is slow, and the product for obtaining point
Son amount distribution is narrow, and anti-freezing property is high, after mix with base catalyst KOH, neutralized original base catalyst it is caused
Molecular weight of product distribution is relatively wide, the deficiency easily frozen, the molecular weight of product point obtained using the mixed catalyst of suitable ratio
Cloth is suitable, and anti-freezing property is high；In addition low-temp reaction is controlled during ethoxylation, reaction terminates rear proper extension degassing time
To 1 hour, so as to reduce low-boiling by-products and penetrating odor in product, finally cause fatty alcohol emulsifying agent congealing point than common
10 DEG C or so of fatty alcohol emulsifying agent reduction；Smell is also similar with mill run without excitant, and product quality has greatly improved,
So as to also ensure that the quality requirement of downstream product.
Finally it is pointed out that above example is only the more representational example of the present invention.Obviously, technology of the invention
Scheme is not limited to above-described embodiment, can also there is many deformations.One of ordinary skill in the art can be from disclosed by the invention
All deformations that content is directly derived or associated, are considered as protection scope of the present invention.
Claims (3)
1. a kind of frost resistance emulsifying agent, it is characterised in that its reaction supplementary material includes：C12-14 fatty alcohols, alkaline mixed catalytic
Agent, oxirane；On the basis of the weight of product：C12-14 fatty alcohols 58.0%~67.0%, alkaline mixed catalyst 0.5%
~1.2%, oxirane 33.0%~42.0%, the alkaline mixed catalyst includes base catalyst and alkaline earth catalyst.
2. a kind of frost resistance emulsifying agent according to claim 1, it is characterised in that the alkali in the alkaline mixed catalyst
Property catalyst be KOH, alkaline earth catalyst be Ba (OH)2, wherein KOH and Ba (OH)2Ratio be 1:1~3.
3. the production technology of the frost resistance emulsifying agent described in a kind of claim 1-2, it is characterised in that comprise the following steps：First
It is heated to 120 DEG C~140 DEG C after C12-14 fatty alcohols are mixed with alkaline mixed catalyst, vacuum dehydration, after the completion of dehydration then
It is cooled to 90 DEG C of rear substitution nitrogen three times, oxirane is slowly added into reactor and the reaction of C12-14 fatty alcohols, control
Temperature after oxirane addition reaches technological requirement, closes oxirane valve between 90-100 DEG C, waits to continue to react one
The section time, pressure and temperature no longer fluctuates and is cooled to 70 DEG C in reactor, then is de-gassed treatment to material in reactor, degassing
Process time extends to 1 hour.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611234098.2A CN106750246A (en) | 2016-12-28 | 2016-12-28 | A kind of frost resistance emulsifying agent and its production technology |
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|---|---|---|---|
| CN201611234098.2A CN106750246A (en) | 2016-12-28 | 2016-12-28 | A kind of frost resistance emulsifying agent and its production technology |
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| CN106750246A true CN106750246A (en) | 2017-05-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114369954A (en) * | 2021-12-30 | 2022-04-19 | 桐乡市恒隆化工有限公司 | Preparation method of antifreezing emulsifier for spinning sizing |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220144A (en) * | 2008-01-24 | 2008-07-16 | 中国石油技术开发公司 | Modified synergistic method of multi-block polyether |
| CN101775115A (en) * | 2010-01-06 | 2010-07-14 | 上海应用技术学院 | Polyurethane elastomer with lateral chain containing fluoroalkyl and preparation method thereof |
| CN102477154A (en) * | 2012-02-28 | 2012-05-30 | 三江化工有限公司 | Preparation method of fatty alcohol polyoxyethylene ether |
-
2016
- 2016-12-28 CN CN201611234098.2A patent/CN106750246A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220144A (en) * | 2008-01-24 | 2008-07-16 | 中国石油技术开发公司 | Modified synergistic method of multi-block polyether |
| CN101775115A (en) * | 2010-01-06 | 2010-07-14 | 上海应用技术学院 | Polyurethane elastomer with lateral chain containing fluoroalkyl and preparation method thereof |
| CN102477154A (en) * | 2012-02-28 | 2012-05-30 | 三江化工有限公司 | Preparation method of fatty alcohol polyoxyethylene ether |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114369954A (en) * | 2021-12-30 | 2022-04-19 | 桐乡市恒隆化工有限公司 | Preparation method of antifreezing emulsifier for spinning sizing |
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Application publication date: 20170531 |
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