CN106008947B - A kind of succinate sulfate and its synthetic method - Google Patents
A kind of succinate sulfate and its synthetic method Download PDFInfo
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- CN106008947B CN106008947B CN201610347342.XA CN201610347342A CN106008947B CN 106008947 B CN106008947 B CN 106008947B CN 201610347342 A CN201610347342 A CN 201610347342A CN 106008947 B CN106008947 B CN 106008947B
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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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/91—Polymers modified by chemical after-treatment
- C08G63/914—Polymers modified by chemical after-treatment derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/918—Polycarboxylic acids and polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
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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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/52—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
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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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/66—Polyesters containing oxygen in the form of ether groups
- C08G63/668—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/676—Polyesters containing oxygen in the form of ether groups derived from polycarboxylic acids and polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
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Abstract
A kind of synthetic method of succinate sulfate is to add in binary acid or acid anhydrides, dihydric alcohol and catalyst in reactor after reacting, then the reaction was continued under reduced pressure to acid value it is constant when, obtain amber acid diester；Will binary acid or acid anhydrides, dihydric alcohol, catalyst and water entrainer add in reactor reaction to acid value it is constant when, obtain amber acid polyester；Amber acid diester or amber acid polyester with preparation after gaseous sulfur trioxide and dry air Hybrid Heating is passed through simultaneously in film sulfonation reactor and carries out sulfating reaction, obtains amber acid diester sulfate or amber acid polyester sulfate.The advantages of present invention has specific structure, and sulphonation rate is high, energy conservation and environmental protection.
Description
Technical field
The present invention relates to a kind of succinate sulfate and its synthetic methods.
Background technology
Succinate sulfate surfactant is a kind of anionic and nonionic type high molecular surfactant, it disperses in pigment
In stabilization process, effective steric hindrance repulsion and electrostatic repulsion are capable of providing, dispersion stabilization is made to be significantly better than traditional surface and is lived
Property agent, there is potential application value in the various fields such as pigment, ink and plastics.
China starts late to the research of macromolecule dispersing agent, and China also develops some macromolecule dispersing agent product in recent years
Kind, but dispersion effect is undesirable, product also non-seriation.Up to the present, the macromolecule dispersing agent developed is mainly used for non-
Disperse in aqueous systems or to organic pigment in aqueous systems, and be used for the macromolecule point disperseed in water-based system to inorganic pigment
The research of powder is less.Therefore high molecular surfactant of the exploitation with specific structure, and study inorganic pigment, ink etc. and exist
Dispersion performance in aqueous systems has very important significance.
In addition, the synthesis of succinate sulfate generally uses two-step method.First, using dihydric alcohol and maleic anhydride as raw material
Double esterification or polycondensation product is made；Then target product is synthesized through sulfating reaction again.The sulfonating agent and process conditions of use
Difference, the quality of sintetics also differ.As Rajesh H.Vekariya (RSC Adv., 2015,5,49006) are reported
Using chlorosulfonic acid come sulfuric acid polyethylene glycol (PEG-OSO3H), which not only generates spent acid, pollutes environment, is added to
This, etching apparatus, it is also necessary to which solvent causes product impure, industrially using less.
The content of the invention
The purpose of the present invention is to solve the decentralized stable problem in water-based system such as inorganic pigment, providing one kind has
Specific structure, and sulphonation rate is high, energy-saving and environment-friendly succinate sulfate and its synthetic method.
Succinate sulfate provided by the invention is divided into two kinds, and molecular structural formula is as follows：
First, amber acid diester sulfate
Wherein, n=22-135
2nd, amber acid polyester sulfate
Wherein, R=-(CH2CH2O)m-, m=0,1,2,8n=17-23.
The synthetic method of succinate sulfate provided by the invention, includes the following steps：
(1) synthesis of succinate
(1) synthesis of amber acid diester：Binary acid or acid anhydrides, dihydric alcohol and catalyst are added in reactor, stirred strongly
It mixes down, after being warming up to 80-100 DEG C of reaction 50-60min, is warming up to 140-170 DEG C under reduced pressure, the reaction was continued to acid value not
During change, stop reaction；Wherein, binary acid or acid anhydrides：The molar ratio of dihydric alcohol is 1:2-2.5；Catalyst amount is the matter that always feeds intake
The 0.5-2% of amount；After reaction, amber acid diester is obtained；
(2) synthesis of amber acid polyester：Binary acid or acid anhydrides, dihydric alcohol, catalyst and water entrainer are added in reactor,
Under strong stirring, 80-100 DEG C of reaction 50-60min is warming up to, then heats to 180-200 DEG C, it is constant to acid value that the reaction was continued
When, stop reaction；Wherein, binary acid or acid anhydrides：The molar ratio of dihydric alcohol is 1:1-1.2；Catalyst amount is the quality that always feeds intake
1-3%；After reaction, vacuum distillation removes water entrainer, obtains amber acid polyester；
(2) synthesis of succinate sulfate
Gaseous sulfur trioxide with dew point less than -60 DEG C of dry airs is mixed, and sulfur trioxide volume is made to account for total gas
2-10%, the amber acid diester or amber acid polyester that mixed gas is heated to preparing with step (1) after 70-140 DEG C are passed through simultaneously
It carries out sulfating reaction in film sulfonation reactor, controls rubbing for amber acid diester or amber acid polyester and the sulfur trioxide that is passed through
You are than being 1:2-3, and controlling reaction temperature is reacted at 20-80 DEG C；After reaction, then aging 30-60min uses lye
To product be neutralized to pH as 7-9, rotary evaporation removes water, obtains amber acid diester sulfate or amber acid polyester sulfuric acid
Salt.
Binary acid or acid anhydrides in step (1) as described above：The molar ratio of dihydric alcohol most preferably 1:2-2.1；The use of catalyst
Amount is preferably that raw material always feeds intake the 1-2% of quality.
Catalyst in step (1) as described above includes：P-methyl benzenesulfonic acid, phosphorous acid or antimony glycol etc..
Dihydric alcohol in step (1) as described above includes：PEG1000, PEG2000, PEG6000 etc., but molecular weight cannot
Big again, if molecular weight is too big, carbonization can occur at high temperature makes color very deep.
Binary acid in step (1) as described above is fumaric acid, glutaconate etc.；Acid anhydrides is maleic anhydride, four
Hydrogenated phthalic anhydride etc..
Binary acid or acid anhydrides in step (2) as described above：The molar ratio of dihydric alcohol most preferably 1:1.1-1.2；Catalyst is used
Measure the 1-2% for the quality that always feeds intake for raw material.
Water entrainer in step (2) as described above includes：Toluene, dimethylbenzene or hexamethylene etc., water entrainer dosage are raw material
The 8-15% of gross mass.
Dihydric alcohol in step (2) as described above includes：Ethylene glycol (EG), diethylene glycol (DEG) (DEG), triethylene glycol (TEG),
The dihydric alcohol of the low molecular weights such as PEG400, if molecular weight polyethylene glycol is larger, then without dehydration polymerization after monoesters is formed
But the polymerization of double bond occurs, so as to form the elastomer of three-dimensional-structure.
Catalyst in step (2) as described above includes：P-methyl benzenesulfonic acid, phosphorous acid or antimony glycol.
Binary acid in step (2) as described above is fumaric acid, glutaconate etc.；Acid anhydrides is maleic anhydride, tetrahydrochysene
Change phthalic anhydride etc..
The gas concentration optimum volume ratio of sulfur trioxide is 4-8% in step (2) mixed gas as described above.
The molar ratio of organic matter and gaseous sulfur trioxide most preferably 1 in step (2) as described above:2-2.5.
Lye in step (2) as described above includes sodium hydroxide, potassium hydroxide, ammonium hydroxide, monomethyl amine or three ethyl alcohol
Amine.
The present invention is by esterification, polycondensation reaction, then through sulfur trioxide sulphation by binary acid (or acid anhydrides) and dihydric alcohol
Succinate sulfuric ester is prepared in reaction, and anion-nonionic type high molecular surfactant-amber is obtained finally by acid-base neutralization
Acid esters sulfate.The type surfactant has both the group of anion and nonionic surfactant, combine anion with
Non-ionic advantage so that the surfactant has stable dispersed, relatively low foaming power and foam stability, can be extensive
Applied in the systems such as textile printing pigment, water paint and water-based ink.
The method of ambroin acid esters sulfate of the present invention, advantage are：1) it is binary acid (or acid anhydrides) and dihydric alcohol is first
Obtain anionic and nonionic type surfactant through esterification, polycondensation, sulphation and neutralization reaction, with strong water-soluble, good point
The advantages that dissipating property.2) target product is prepared by gaseous sulfur trioxide sulphation method, reaction process is easy to operate, conversion ratio
Height, reaction rate are fast.3) reaction process generates without spent acid, is corrosion-free to equipment, having excellent Environmental compatibility.
Description of the drawings
Fig. 1 is the infrared spectrum of the final product amber acid polyester sulfate of the embodiment of the present invention 4.
Specific embodiment
Embodiment 1
By the maleic anhydride of 9.80g (0.10mol), the polyethylene glycol PEG1000 and 4.40g of 210.0g (0.21mol)
P-methyl benzenesulfonic acid be added in the four-hole boiling flask with thermometer, electric blender and water knockout drum, under strong stirring, be warming up to
80 DEG C reaction 50min after, 140 DEG C are warming up under reduced pressure, the reaction was continued to acid value it is constant when, stop reaction, obtain Malaysia
Acid diester glycol.Gaseous sulfur trioxide with dew point less than -60 DEG C of dry airs is mixed, sulfur trioxide volume is made to account for total gas
8%, mixed gas be heated to 70 DEG C after with maleic acid diester glycol be passed through simultaneously in film sulfonation reactor carry out sulphation it is anti-
Should, it is 1 to control the molar ratio of organic matter and gaseous sulfur trioxide:2.5, temperature is reacted at 20 DEG C, after reaction, aging
30min, it is 8 that product, which is carried out being neutralized to pH, with sodium hydroxide solution, and rotary evaporation removes water, obtains maleic acid diester sulfuric acid
Sodium.It measuring wherein anionic Active content and reaches 60%, sulphates content 0.28%, unsulfonated material content is 1.43%,
Polymer is in the dispersion performance test of barium sulfate powder, barium sulfate suspensibility is up to 90%.
Embodiment 2
By the maleic anhydride of 4.90g (0.05mol), 230.0g (0.115mol) polyethylene glycol PEG2000 and
The p-methyl benzenesulfonic acid of 2.35g is added in the four-hole boiling flask with thermometer, electric blender and water knockout drum, under strong stirring,
After being warming up to 90 DEG C of reaction 60min, 150 DEG C are warming up under reduced pressure, the reaction was continued to acid value be basically unchanged when, stop anti-
Should, obtain maleic acid diester glycol.Gaseous sulfur trioxide with dew point less than -60 DEG C of dry airs is mixed, makes sulfur trioxide body
Than being 6%, mixed gas after being heated to 80 DEG C is passed through with maleic acid diester glycol in film sulfonation reactor and carries out sulphur product simultaneously
Acidification reaction, it is 1 to control the molar ratio of organic matter and gaseous sulfur trioxide:2.2, control temperature is reacted at 30 DEG C, reaction knot
Shu Hou, aging 40min, it is 8 that product, which is carried out being neutralized to pH, with sodium hydroxide solution, and rotary evaporation removes water, obtains maleic acid
Ethoxylate Bis-sodium Sulfate.It measures wherein anionic Active content and reaches 65%, sulphates content 0.35%, unsulfonated material content is
1.62%, in polymer in the dispersion performance test of barium sulfate powder, barium sulfate suspensibility is up to 88%.
Embodiment 3
By the maleic anhydride of 2.45g (0.025mol), 375.0g (0.0625mol) polyethylene glycol PEG6000 and
The p-methyl benzenesulfonic acid of 1.89g is added in the four-hole boiling flask with thermometer, electric blender and water knockout drum, under strong stirring,
After being warming up to 100 DEG C of reaction 55min, 170 DEG C are warming up under reduced pressure, the reaction was continued to acid value be basically unchanged when, stop anti-
Should, obtain maleic acid diester glycol.Gaseous sulfur trioxide with dew point less than -60 DEG C of dry airs is mixed, makes sulfur trioxide body
Than being 10%, mixed gas after being heated to 100 DEG C is passed through with maleic acid diester glycol in film sulfonation reactor and carries out product simultaneously
Sulfating reaction, it is 1 to control the molar ratio of organic matter and gaseous sulfur trioxide:2, control temperature is reacted at 40 DEG C, reaction knot
Shu Hou, aging 50min, it is 8 that product, which is carried out being neutralized to pH, with sodium hydroxide solution, and rotary evaporation removes water, obtains maleic acid
Ethoxylate Bis-sodium Sulfate.It measures wherein anionic Active content and reaches 62%, sulphates content 0.25%, unsulfonated material content is
1.55%, in polymer in the dispersion performance test of barium sulfate powder, barium sulfate suspensibility is up to 92%.
Embodiment 4
By the maleic anhydride of 30.0g (0.30mol), polyethylene glycol PEG400,13.12g diformazan of 134.1g (0.33mol)
The p-methyl benzenesulfonic acid of benzene and 3.282g are added in the four-hole boiling flask with thermometer, electric blender and water knockout drum, strongly
Under stirring, be warming up to 100 DEG C of reactions 1 it is small when, then heat to 180 DEG C, the reaction was continued to acid value be basically unchanged when, stop anti-
Should, vacuum distillation removes water entrainer, obtains maleic polyester glycol.Gaseous sulfur trioxide and dew point is dry less than -60 DEG C empty
Gas mixes, and makes sulfur trioxide volume ratio for 4%, and mixed gas with maleic polyester glycol is passed through film simultaneously after being heated to 140 DEG C
Sulfating reaction is carried out in formula sulfonation reactor, it is 1 to control the molar ratio of organic matter and gaseous sulfur trioxide:3, control temperature exists
It is reacted at 70 DEG C, after reaction, aging 30min, it is 8 that product, which is carried out being neutralized to pH, with sodium hydroxide solution, rotary evaporation
Water is removed, obtains maleic polyester sodium sulphate.It measures wherein anionic Active content and reaches 65%, sulphates content
0.26%, unsulfonated material content is 1.21%, in polymer tests the dispersion performance of barium sulfate powder, barium sulfate suspensibility
Up to 89%.
Embodiment 5
By the maleic anhydride of 30.0g (0.30mol), the triethylene glycol of 54.25g (0.36mol), 10.11g dimethylbenzene and
The p-methyl benzenesulfonic acid of 0.84g is added in the four-hole boiling flask with thermometer, electric blender and water knockout drum, under strong stirring,
Be warming up to 80 DEG C reaction 55min, then heat to 190 DEG C, the reaction was continued to acid value be basically unchanged when, stop reaction, decompression steam
Water entrainer is removed in distillation, obtains maleic polyester glycol.Gaseous sulfur trioxide with dew point less than -60 DEG C of dry airs is mixed, is made
Sulfur trioxide volume ratio is 2%, and mixed gas is passed through membrane-type sulfonation with maleic polyester glycol after being heated to 130 DEG C and reacts simultaneously
Sulfating reaction is carried out in device, it is 1 to control the molar ratio of organic matter and gaseous sulfur trioxide:2.7, control temperature is anti-at 80 DEG C
Should, after reaction, rotary evaporation remove water entrainer, aging 50min, product is carried out being neutralized to pH with sodium hydroxide solution be
8, rotary evaporation removes water, obtains maleic polyester sodium sulphate.It measures wherein anionic Active content and reaches 70%, sulfate
Content 0.15%, unsulfonated material content are 1.04%, in polymer in the dispersion performance test of barium sulfate powder, barium sulfate hangs
Floating rate is up to 90%.
Embodiment 6
By the maleic anhydride of 49.0g (0.50mol), the diethylene glycol (DEG) of 53.06g (0.5mol), 16.33g dimethylbenzene and
The p-methyl benzenesulfonic acid of 3.06g is added in the four-hole boiling flask with thermometer, electric blender and water knockout drum, under strong stirring,
Be warming up to 90 DEG C reaction 50min, then heat to 200 DEG C, the reaction was continued to acid value be basically unchanged when, stop reaction, decompression steam
Water entrainer is removed in distillation, obtains maleic polyester glycol.Gaseous sulfur trioxide with dew point less than -60 DEG C of dry airs is mixed, is made
Sulfur trioxide volume ratio is 5%, and mixed gas is passed through membrane-type sulfonation with maleic polyester glycol after being heated to 120 DEG C and reacts simultaneously
Sulfating reaction is carried out in device, it is 1 to control the molar ratio of organic matter and gaseous sulfur trioxide:2.3, control temperature is anti-at 50 DEG C
Should, after reaction, aging 60min, it is 8 that product, which is carried out being neutralized to pH, with sodium hydroxide solution, and rotary evaporation removes water, obtains
To maleic polyester sodium sulphate.It measures wherein anionic Active content and reaches 63%, sulphates content 0.20%, unsulfonated material
Content is 1.56%, in polymer in the dispersion performance test of barium sulfate powder, barium sulfate suspensibility is up to 85%.
Embodiment 7
By the maleic anhydride of 49.0g (0.50mol), the ethylene glycol of 37.24g (0.60mol), 17.25g dimethylbenzene and
The p-methyl benzenesulfonic acid of 1.725g is added in the four-hole boiling flask with thermometer, electric blender and water knockout drum, under strong stirring,
Be warming up to 100 DEG C reaction 1 it is small when, then heat to 190 DEG C, the reaction was continued to acid value be basically unchanged when, stop reaction, decompression steam
Water entrainer is removed in distillation, obtains maleic polyester glycol.Gaseous sulfur trioxide with dew point less than -60 DEG C of dry airs is mixed, is made
Sulfur trioxide volume ratio is 7%, and mixed gas is passed through membrane-type sulfonation with maleic polyester glycol after being heated to 110 DEG C and reacts simultaneously
Sulfating reaction is carried out in device, it is 1 to control the molar ratio of organic matter and gaseous sulfur trioxide:2.9, control temperature is anti-at 60 DEG C
Should, after reaction, aging 40min, it is 8 that product, which is carried out being neutralized to pH, with sodium hydroxide solution, and rotary evaporation removes water, obtains
To maleic polyester sodium sulphate.It measures wherein anionic Active content and reaches 63%, sulphates content 0.12%, unsulfonated material
Content is 0.89%, in polymer in the dispersion performance test of barium sulfate powder, barium sulfate suspensibility is up to 93%.
Claims (19)
1. a kind of succinate sulfate, it is characterised in that molecular structural formula is as follows：
Wherein, n=22-135.
2. a kind of succinate sulfate, it is characterised in that molecular structural formula is as follows：
Wherein, R=-(CH2CH2O)m-, m=1,2,8, n=17-23.
3. a kind of synthetic method of succinate sulfate as claimed in claim 1 or 2, it is characterised in that including walking as follows
Suddenly：
(1) synthesis of succinate
(1) synthesis of amber acid diester：Binary acid or acid anhydrides, dihydric alcohol and catalyst are added in reactor, under strong stirring,
Be warming up to 80-100 DEG C reaction 50-60min after, be warming up to 140-170 DEG C under reduced pressure, the reaction was continued to acid value it is constant when,
Stop reaction；Wherein, binary acid or acid anhydrides：The molar ratio of dihydric alcohol is 1:2-2.5；Catalyst amount is the quality that always feeds intake
0.5-2%；After reaction, amber acid diester is obtained；
(2) synthesis of amber acid polyester：Binary acid or acid anhydrides, dihydric alcohol, catalyst and water entrainer are added in reactor, strongly
Under stirring, be warming up to 80-100 DEG C reaction 50-60min, then heat to 180-200 DEG C, the reaction was continued to acid value it is constant when, stop
Only react；Wherein, binary acid or acid anhydrides：The molar ratio of dihydric alcohol is 1:1-1.2；Catalyst amount is the 1- of quality of always feeding intake
3%；After reaction, vacuum distillation removes water entrainer, obtains amber acid polyester；
(2) synthesis of succinate sulfate
Gaseous sulfur trioxide with dew point less than -60 DEG C of dry airs is mixed, and sulfur trioxide volume is made to account for the 2- of total gas
10%, the amber acid diester or amber acid polyester that mixed gas is heated to preparing with step (1) after 70-140 DEG C are passed through film simultaneously
Sulfating reaction is carried out in formula sulfonation reactor, controls mole of amber acid diester or amber acid polyester and the sulfur trioxide being passed through
Than for 1:2-3, and controlling reaction temperature is reacted at 20-80 DEG C；After reaction, aging 30-60min, then with lye pair
Product be neutralized to pH as 7-9, and rotary evaporation removes water, obtains amber acid diester sulfate or amber acid polyester sulfate.
4. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that two in the step (1)
First acid or acid anhydrides：The molar ratio of dihydric alcohol is 1:2-2.1.
5. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that urged in the step (1)
The dosage of agent always feeds intake the 1-2% of quality for raw material.
6. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (1)
Catalyst includes p-methyl benzenesulfonic acid, phosphorous acid or antimony glycol.
7. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (1)
Dihydric alcohol includes PEG1000, PEG2000 or PEG6000.
8. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (1)
Binary acid is fumaric acid.
9. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that sour in the step (1)
Acid anhydride is maleic anhydride.
10. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (2)
Binary acid or acid anhydrides：The molar ratio of dihydric alcohol is 1:1.1-1.2.
11. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (2)
Catalyst amount always feeds intake the 1-2% of quality for raw material.
12. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (2)
Water entrainer include toluene, dimethylbenzene or hexamethylene, water entrainer dosage be raw material gross mass 8-15%.
13. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (2)
Dihydric alcohol include ethylene glycol, diethylene glycol (DEG) or PEG400.
14. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (2)
Catalyst include p-methyl benzenesulfonic acid, phosphorous acid or antimony glycol.
15. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (2)
Binary acid be fumaric acid.
16. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (2)
Acid anhydrides is maleic anhydride.
17. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that the step (2) is mixed
The gas concentration volume ratio for closing sulfur trioxide in gas is 4-8%.
18. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (2)
Amber acid diester or the molar ratio of amber acid polyester and gaseous sulfur trioxide are 1:2-2.5.
19. a kind of synthetic method of succinate sulfate as claimed in claim 3, it is characterised in that in the step (2)
Alkali include sodium hydroxide, potassium hydroxide, ammonium hydroxide, monomethyl amine or triethanolamine.
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| "磺酸盐型高分子表面活性剂的合成及性能";胡守印;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20111215(第12期);B016-130 * |
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