CN103304736A - Preparation method of water soluble dispersant - Google Patents
Preparation method of water soluble dispersant Download PDFInfo
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- CN103304736A CN103304736A CN2013102324119A CN201310232411A CN103304736A CN 103304736 A CN103304736 A CN 103304736A CN 2013102324119 A CN2013102324119 A CN 2013102324119A CN 201310232411 A CN201310232411 A CN 201310232411A CN 103304736 A CN103304736 A CN 103304736A
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Abstract
The invention provides a preparation method of a water soluble dispersant. The preparation method is characterized by comprising the following steps of: adding 40%-60% of C4 component, 1%-18% of maleic anhydride and 0.1%-4% of initiator to a high-pressure kettle, wherein the weight of a solvent is 0.4-5 times of the total weight of the raw materials and the sum of the weight percentages of all the raw materials is 100%; after nitrogen displacement, maintaining the pressure of the reaction kettle in the range from 0.3 to 2 MPa, and maintaining the reaction temperature in the range from 40 to 150 DEG C for 1-5 hours; after the reaction is completed, collecting residual gas in the high-pressure kettle to an auxiliary gas bottle, after the product is subjected to the aftertreatment steps of distillation, filtering, performing drip washing by using a drip washing agent, drying the product in a vacuum oven at a temperature ranging from 40 to 150 DEG C for 2-36 hours, and then hydrolyzing under an alkaline condition, thereby obtaining the water soluble dispersant of a series of molecular weight distributions, wherein the molecular weight distribution of the product ranges from 3000 to 100000 Mn.
Description
Technical field
The invention belongs to the macromolecular material production technical field, relate to a kind of preparation method of water soluble dispersing agent.
A kind of preparation method who utilizes C4 component, maleic anhydride polymerization to produce macromolecule dispersing agent.
Background technology
Be the macromolecular material of material copolymerization with the maleic anhydride, hydroxy number is many than the polyacrylic Scale inhibitors in its structure, therefore has good thermostability and resistance CaCO
3And CaSO
4The dirt performance has application widely in water treatment field.Simultaneously have the polar functionalities group because of it, be widely used in the compound of plastics, metal, paper as jointing material; Compatilizer as the macromolecular material blend also is used widely in the engineering plastics field.
At the particular requirement of macromolecular material, utilize the maleic anhydride modified focus that numerous research and development institutions pay close attention to that becomes in recent years.Maleic anhydride modified is to be monomer with the maleic anhydride, carries out grafting with some materials under suitable temperature, and monomer can be alkenes compounds, also olefin(e) acid compounds.Maleic anhydride grafts owing to contain polar group that maleic anhydride provides and the non-polar group of alkene simultaneously, therefore can be widely used in PA, PP, PE modification, and wood is moulded industries such as industry and hot melt adhesive.
Patent CN200810038559.8 has introduced a kind of method of maleic anhydride graft polyisobutene.This method is used maleic anhydride and iso-butylene, initiator and oxidation inhibitor simultaneously in the presence of, by the solvent thermal preparation method, prepare a kind of polymer toughner.
Patent CN96115574.4, introduced the method for a kind of maleic anhydride and isobutene reaction synthetic resins, this method is used maleic anhydride and iso-butylene, under the initiation with Diisopropyl azodicarboxylate or benzoyl peroxide, 50 ~ 90 ℃ of temperature, polymerization pressure 0.05 ~ 1.0MPa in 2 ~ 10 hours reaction times, adopts solvent method synthetic resins in autoclave.
By inquiring about domestic patent as can be known, though the patent application that utilizes of existing maleic anhydride and various C4 components proposes, content relates to functional resin, resin flexibilizer etc., but there is no the report that utilizes maleic anhydride and this paper indication C4 component to prepare water soluble dispersing agent so far.
Summary of the invention
The objective of the invention is to utilize the method for the synthetic a kind of new type water-solubility dispersion agent of specific C4 component in maleic anhydride and the petroleum fractions.
The present invention is a kind of preparation method of water soluble dispersing agent, it is characterized in that: adopt following step:
The C4 component that adds in autoclave is 40% ~ 60%, maleic anhydride is 1% ~ 18%, initiator is 0.1% ~ 4%, and solvent quality is 0.4 ~ 5 times of raw material summation, and each raw material weight per-cent total amount sum is 100%.Behind the nitrogen replacement, reactor pressure maintains 0.3 ~ 2MPa, and temperature of reaction is kept 1 ~ 5h under 40 ~ 150 ℃.Reaction finishes residual gas in the autoclave is collected into bailout bottle, product is through post-processing steps such as distillation, filtration, eluent drip washing, 40 ~ 150 ℃ of vacuum drying oven dryings 2 ~ 36 hours, hydrolysis under alkaline condition again, namely obtain the water soluble dispersing agent of a series of molecular weight distribution, molecular weight of product distribution range 3000 ~ 100000Mn.
According to described preparation method, it is characterized in that described raw material C4 component is pressurized liquefied back charging, the C4 component added in the autoclave after charging adopted the continuously feeding mode to liquefy; Described raw material C4 component is a kind of of butene-1, butene-2, iso-butylene and divinyl, or its blending ingredients; Described monomer ratio weight ratio is maleic anhydride: C4=1:1 ~ 5:1;
According to described preparation method, it is characterized in that described initiator is a kind of of Diisopropyl azodicarboxylate, benzoyl peroxide, dicumyl peroxide, the peroxidation tert-butyl ester, peroxidation diisobutyl ester, peroxidized t-butyl perbenzoate or peroxidation isopropyl ester, or its mixed solvent;
Described solvent is a kind of of tetrahydrofuran (THF), ethylene glycol, the trimethyl carbinol, normal hexane, benzene,toluene,xylene, ethyl acetate, butylacetate, butanone or deionized water, or its mixed solvent.
Described eluent is a kind of in methylene dichloride, ethylene dichloride, acetone, ethanol, the tetracol phenixin, or its mixed solvent.
According to described preparation method, it is characterized in that 50 ~ 130 ℃ of range of reaction temperature; Reaction pressure scope 0.5 ~ 1.8MPa; Reaction time range 1 ~ 4.5h.
According to described preparation method, it is characterized in that the range of molecular weight distributions 4000 ~ 90000Mn of product.
Embodiment
Embodiment one
Add the maleic anhydride (technical grade) of 30g in autoclave, 5g benzoyl peroxide (BPO) and 200g normal hexane stirring and dissolving are even.Keep nitrogen atmosphere behind the nitrogen replacement 1 time, nitrogen pressure is to 1.0MPa, be warming up to 100 ℃, inject divinyl 95g in autoclave during this time, reacted 5 hours, be cooled to room temperature, reduce the still internal pressure and to normal pressure, drive still, product solid-liquid mixed phase, reducing pressure distills out normal hexane under-0.80MPa, get crude product; Crude product gets the white powder solid product behind acetone drip washing, ethyl alcohol recrystallization, molecular weight is 5000 ~ 10000; Final product was through 80 ℃ of vacuum drying oven oven dry 4 hours, and hydrolysis under alkaline condition more namely gets water soluble dispersing agent of the present invention.
Embodiment two
The maleic anhydride (technical grade) that in autoclave, adds 50g, the 4g dicumyl peroxide, the 200g trimethyl carbinol and 50g ethylene glycol, the mixing stirring and dissolving is even.Keep nitrogen atmosphere behind the nitrogen replacement 1 time, nitrogen pressure is to 1.9MPa, be warming up to 110 ℃, inject divinyl 150g in autoclave during this time, reacted 4 hours, be cooled to room temperature, reduce the still internal pressure and to normal pressure, drive still, product solid-liquid mixed phase, the distilling off solvent trimethyl carbinol and the ethylene glycol under-0.80MPa that reduces pressure gets crude product; Crude product gets the white powder solid product behind acetone drip washing, ethyl alcohol recrystallization, molecular weight is 10000 ~ 50000; Final product was through 80 ℃ of vacuum drying oven oven dry 8 hours, and hydrolysis under alkaline condition more namely gets water soluble dispersing agent of the present invention.
Embodiment three
Add the maleic anhydride (technical grade) of 50g in autoclave, 5g Diisopropyl azodicarboxylate (AIBN) and 200g trimethyl carbinol stirring and dissolving are even.Keep nitrogen atmosphere behind the nitrogen replacement 1 time, nitrogen pressure is to 1.5MPa, be warming up to 110 ℃, inject divinyl 148g in autoclave during this time, reacted 5 hours, be cooled to room temperature, reduce the still internal pressure and to normal pressure, drive still, product solid-liquid mixed phase, reducing pressure distills out the trimethyl carbinol under-0.80MPa, get crude product; Crude product gets the white powder solid product behind acetone drip washing, ethyl alcohol recrystallization, molecular weight is 4000 ~ 8000; Final product was through 80 ℃ of vacuum drying oven oven dry 6 hours, and hydrolysis under alkaline condition more namely gets water soluble dispersing agent of the present invention.
Claims (4)
1. the preparation method of a water soluble dispersing agent is characterized in that: adopt following step:
The C4 component that adds in autoclave is 40% ~ 60%, maleic anhydride is 1% ~ 18%, initiator is 0.1% ~ 4%, and solvent quality is 0.4 ~ 5 times of raw material summation, and each raw material weight per-cent total amount sum is 100%; Behind the nitrogen replacement, reactor pressure maintains 0.3 ~ 2MPa, and temperature of reaction is kept 1 ~ 5h under 40 ~ 150 ℃; Reaction finishes residual gas in the autoclave is collected into bailout bottle, product is through distillation, filtration, eluent drip washing post-processing step, 40 ~ 150 ℃ of vacuum drying oven dryings 2 ~ 36 hours, hydrolysis under alkaline condition again, namely obtain the water soluble dispersing agent of a series of molecular weight distribution, molecular weight of product distribution range 3000 ~ 100000Mn.
2. preparation method according to claim 1 is characterized in that: described raw material C4 component is pressurized liquefied back charging, and charging adopts the continuously feeding mode will liquefy in the back C4 component adding autoclave; Described raw material C4 component is a kind of of butene-1, butene-2, iso-butylene and divinyl, or its blending ingredients; Described monomer ratio weight ratio is maleic anhydride: C4=1:1 ~ 5:1.
3. preparation method according to claim 1, it is characterized in that described initiator is a kind of of Diisopropyl azodicarboxylate, benzoyl peroxide, dicumyl peroxide, the peroxidation tert-butyl ester, peroxidation diisobutyl ester, peroxidized t-butyl perbenzoate or peroxidation isopropyl ester, or its mixed solvent;
Described solvent is a kind of of tetrahydrofuran (THF), ethylene glycol, the trimethyl carbinol, normal hexane, benzene,toluene,xylene, ethyl acetate, butylacetate, butanone or deionized water, or its mixed solvent;
Described eluent is a kind of in methylene dichloride, ethylene dichloride, acetone, ethanol, the tetracol phenixin, or its mixed solvent.
4. preparation method according to claim 1 is characterized in that 50 ~ 130 ℃ of range of reaction temperature; Reaction pressure scope 0.5 ~ 1.8MPa; Reaction time range 1 ~ 4.5h; Range of molecular weight distributions 4000 ~ the 90000Mn of product.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104356295A (en) * | 2014-11-13 | 2015-02-18 | 中国海洋石油总公司 | Method for preparing high polymer bonding substrate from mixed C4 fraction |
| CN108624122A (en) * | 2018-06-08 | 2018-10-09 | 奥莱鑫科技股份有限公司 | A kind of environment-friendly type high concentration Neutral writing ink mill base and preparation method thereof |
| CN109160974A (en) * | 2018-07-27 | 2019-01-08 | 天津安浩生物科技有限公司 | A kind of aqueous phase preparation method of maleic anhydride-conjugated diene copolymer |
| CN111484579A (en) * | 2020-04-16 | 2020-08-04 | 陕西科技大学 | High-temperature soluble bridge plug and preparation method thereof |
| CN112094673A (en) * | 2020-09-24 | 2020-12-18 | 蒋云超 | High-temperature dispersing agent for heavy oil deep processing device and preparation and application thereof |
| CN116262803A (en) * | 2021-12-13 | 2023-06-16 | 中国石油化工股份有限公司 | Maleic anhydride-isobutene copolymer microsphere and preparation method and application thereof |
| CN116262802A (en) * | 2021-12-13 | 2023-06-16 | 中国石油化工股份有限公司 | Maleic anhydride-conjugated diene copolymer microsphere, and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1175594A (en) * | 1996-09-05 | 1998-03-11 | 中国石化锦州石油化工公司 | Method for preparing strong water absorbent |
-
2013
- 2013-06-13 CN CN201310232411.9A patent/CN103304736B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1175594A (en) * | 1996-09-05 | 1998-03-11 | 中国石化锦州石油化工公司 | Method for preparing strong water absorbent |
Non-Patent Citations (1)
| Title |
|---|
| 戚银城等: "IBMA树脂的合成与表征", 《高分子材料科学与工程》, no. 2, 31 March 1992 (1992-03-31), pages 38 - 43 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104356295A (en) * | 2014-11-13 | 2015-02-18 | 中国海洋石油总公司 | Method for preparing high polymer bonding substrate from mixed C4 fraction |
| CN108624122A (en) * | 2018-06-08 | 2018-10-09 | 奥莱鑫科技股份有限公司 | A kind of environment-friendly type high concentration Neutral writing ink mill base and preparation method thereof |
| CN109160974A (en) * | 2018-07-27 | 2019-01-08 | 天津安浩生物科技有限公司 | A kind of aqueous phase preparation method of maleic anhydride-conjugated diene copolymer |
| CN111484579A (en) * | 2020-04-16 | 2020-08-04 | 陕西科技大学 | High-temperature soluble bridge plug and preparation method thereof |
| CN112094673A (en) * | 2020-09-24 | 2020-12-18 | 蒋云超 | High-temperature dispersing agent for heavy oil deep processing device and preparation and application thereof |
| CN112094673B (en) * | 2020-09-24 | 2022-03-01 | 蒋云超 | High-temperature dispersing agent for heavy oil deep processing device and preparation and application thereof |
| CN116262803A (en) * | 2021-12-13 | 2023-06-16 | 中国石油化工股份有限公司 | Maleic anhydride-isobutene copolymer microsphere and preparation method and application thereof |
| CN116262802A (en) * | 2021-12-13 | 2023-06-16 | 中国石油化工股份有限公司 | Maleic anhydride-conjugated diene copolymer microsphere, and preparation method and application thereof |
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| CN103304736B (en) | 2015-09-23 |
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Effective date of registration: 20180306 Address after: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Co-patentee after: CNOOC TIANJIN CHEMICAL RESEARCH & DESIGN INSTITUTE CO., LTD. Patentee after: China National Offshore Oil Corporation Co-patentee after: CNOOC Huizhou Petrochemical Co., Ltd. Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Co-patentee before: CNOOC Tianjin Chemical Research & Design Institute Patentee before: China National Offshore Oil Corporation Co-patentee before: Huizhou Refinery Branch, CNOOC Oil & Petrochemicals Co., Ltd. |