CN103304736B - A kind of preparation method of water soluble dispersing agent - Google Patents
A kind of preparation method of water soluble dispersing agent Download PDFInfo
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- CN103304736B CN103304736B CN201310232411.9A CN201310232411A CN103304736B CN 103304736 B CN103304736 B CN 103304736B CN 201310232411 A CN201310232411 A CN 201310232411A CN 103304736 B CN103304736 B CN 103304736B
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Abstract
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 added in autoclave is 40% ~ 60%, maleic anhydride is 1% ~ 18%, initiator is 0.1% ~ 4%, solvent quality is 0.4 ~ 5 times of raw material summation, and each raw material weight per-cent total amount sum is 100%; After nitrogen replacement, reactor pressure maintains 0.3 ~ 2MPa, and temperature of reaction maintains 1 ~ 5h at 40 ~ 150 DEG C; React complete and residual gas in autoclave is collected into bailout bottle, product is through distillation, filtration, eluent drip washing post-processing step, 40 ~ 150 DEG C of vacuum drying oven dryings 2 ~ 36 hours, be hydrolyzed in the basic conditions again, namely the water soluble dispersing agent of a series of molecular weight distribution is obtained, molecular weight of product distribution range 3000 ~ 100000Mn.
Description
Technical field
The invention belongs to macromolecular material production technical field, relate to a kind of preparation method of water soluble dispersing agent.
A kind of C4 component, maleic anhydride of utilizing is polymerized the preparation method producing macromolecule dispersing agent.
Background technology
Take maleic anhydride as the macromolecular material of material copolymerization, in its structure, hydroxy number is many compared with polyacrylic Scale inhibitors, therefore has good thermostability and resistance CaCO
3and CaSO
4dirt performance, has a wide range of applications in water treatment field.Because of it, there is polar functional group simultaneously, be widely used in the compound of plastics, metal, paper as jointing material; The compatilizer blended as macromolecular material is also used widely in engineering plastics field.
For the particular requirement of macromolecular material, utilize the maleic anhydride modified focus becoming numerous research and development institution and pay close attention in recent years.Maleic anhydride modified is take maleic anhydride as monomer, and carry out grafting with some materials at a suitable temperature, monomer can be alkenes compounds, may also be olefin(e) acid compounds.Maleic anhydride grafts, due to the non-polar group of the polar group that provides containing maleic anhydride and alkene simultaneously, therefore can be widely used in PA, PP, PE modification, the industry such as industry and hot melt adhesive moulded by wood.
Patent CN200810038559.8, describes a kind of method of maleic anhydride graft polyisobutene.The method uses maleic anhydride and iso-butylene, initiator and oxidation inhibitor simultaneously in the presence of, by solvent thermal preparation method, prepare a kind of macromolecular toughening agent.
Patent CN96115574.4, describe a kind of method of maleic anhydride and isobutene reaction synthetic resins, the method uses maleic anhydride and iso-butylene, with under the initiation of Diisopropyl azodicarboxylate or benzoyl peroxide, temperature 50 ~ 90 DEG C, polymerization pressure 0.05 ~ 1.0MPa, in 2 ~ 10 hours reaction times, adopts solvent method synthetic resins in autoclave.
Known by inquiring about domestic patent, although the patent application that utilizes of existing maleic anhydride and various C4 component proposes, content relates to functional resin, resin flexibilizer etc., but there is no the report utilizing maleic anhydride and this paper indication C4 component to prepare water soluble dispersing agent so far.
Summary of the invention
The object of the invention is to utilize the specific C4 component in maleic anhydride and petroleum fractions to synthesize a kind of method of new type water-solubility dispersion agent.
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 added 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%.After nitrogen replacement, reactor pressure maintains 0.3 ~ 2MPa, and temperature of reaction maintains 1 ~ 5h at 40 ~ 150 DEG C.React complete and residual gas in autoclave is collected into bailout bottle, product is through post-processing steps such as distillation, filtration, eluent drip washing, 40 ~ 150 DEG C of vacuum drying oven dryings 2 ~ 36 hours, be hydrolyzed in the basic conditions again, namely the water soluble dispersing agent of a series of molecular weight distribution is obtained, 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 rear feeding, charging adopts continuously feeding mode to add in autoclave by post liquefaction C4 component; Described raw material C4 component is the one 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 the one of Diisopropyl azodicarboxylate, benzoyl peroxide, dicumyl peroxide, t-butylperbenzoate, peroxidation diisobutyl ester, peroxidized t-butyl perbenzoate or peroxidation isopropyl ester, or its mixed solvent;
Described solvent is the one 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 the one in methylene dichloride, ethylene dichloride, acetone, ethanol, tetracol phenixin, or its mixed solvent.
According to described preparation method, it is characterized in that range of reaction temperature 50 ~ 130 DEG C; 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
In autoclave, add the maleic anhydride (technical grade) of 30g, 5g benzoyl peroxide (BPO) and 200g normal hexane stirring and dissolving even.Nitrogen atmosphere is kept after nitrogen replacement 1 time, nitrogen pressurization is to 1.0MPa, be warming up to 100 DEG C, period injects divinyl 95g in autoclave, reacts 5 hours, is cooled to room temperature, still is driven after reducing still internal pressure to normal pressure, product solid-liquid mixed phase, reduce pressure distills out normal hexane under-0.80MPa, obtains crude product; Crude product obtains white powder solid product after acetone drip washing, ethyl alcohol recrystallization, and molecular weight is 5000 ~ 10000; Final product dries 4 hours through 80 DEG C of vacuum drying ovens, then is hydrolyzed in the basic conditions, obtains water soluble dispersing agent of the present invention.
Embodiment two
In autoclave, add the maleic anhydride (technical grade) of 50g, 4g dicumyl peroxide, the 200g trimethyl carbinol and 50g ethylene glycol, mix and blend is uniformly dissolved.Nitrogen atmosphere is kept after nitrogen replacement 1 time, nitrogen pressurization is to 1.9MPa, be warming up to 110 DEG C, period injects divinyl 150g in autoclave, reacts 4 hours, is cooled to room temperature, still is driven after reducing still internal pressure to normal pressure, product solid-liquid mixed phase, reduce pressure the distilling off solvent trimethyl carbinol and ethylene glycol under-0.80MPa, obtains crude product; Crude product obtains white powder solid product after acetone drip washing, ethyl alcohol recrystallization, and molecular weight is 10000 ~ 50000; Final product dries 8 hours through 80 DEG C of vacuum drying ovens, then is hydrolyzed in the basic conditions, obtains water soluble dispersing agent of the present invention.
Embodiment three
In autoclave, add the maleic anhydride (technical grade) of 50g, 5g Diisopropyl azodicarboxylate (AIBN) and 200g trimethyl carbinol stirring and dissolving even.Nitrogen atmosphere is kept after nitrogen replacement 1 time, nitrogen pressurization is to 1.5MPa, be warming up to 110 DEG C, period injects divinyl 148g in autoclave, reacts 5 hours, is cooled to room temperature, still is driven after reducing still internal pressure to normal pressure, product solid-liquid mixed phase, reduce pressure distills out the trimethyl carbinol under-0.80MPa, obtains crude product; Crude product obtains white powder solid product after acetone drip washing, ethyl alcohol recrystallization, and molecular weight is 4000 ~ 8000; Final product dries 6 hours through 80 DEG C of vacuum drying ovens, then is hydrolyzed in the basic conditions, obtains water soluble dispersing agent of the present invention.
Claims (3)
1. a preparation method for water soluble dispersing agent, is characterized in that: adopt following step:
The C4 component added 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%; After nitrogen replacement, reactor pressure maintains 0.3 ~ 2MPa, and temperature of reaction maintains 1 ~ 5h at 40 ~ 150 DEG C; React complete and residual gas in autoclave is collected into bailout bottle, product is through distillation, filtration, eluent drip washing post-processing step, 40 ~ 150 DEG C of vacuum drying oven dryings 2 ~ 36 hours, be hydrolyzed in the basic conditions again, namely the water soluble dispersing agent of a series of molecular weight distribution is obtained, molecular weight of product distribution range 3000 ~ 100000Mn; Described raw material C4 component is pressurized liquefied rear feeding, and charging adopts continuously feeding mode to add in autoclave by post liquefaction C4 component; Described raw material C4 component is the one of butene-1, butene-2, divinyl, or its blending ingredients; Described monomer ratio weight ratio is maleic anhydride: C4=1:1 ~ 5:1; .
2. preparation method according to claim 1, it is characterized in that: described initiator is the one of Diisopropyl azodicarboxylate, benzoyl peroxide, dicumyl peroxide, t-butylperbenzoate, peroxidation diisobutyl ester, peroxidized t-butyl perbenzoate or peroxidation isopropyl ester, or its mixed solvent;
Described solvent is the one 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 the one in methylene dichloride, ethylene dichloride, acetone, ethanol, tetracol phenixin, or its mixed solvent.
3. preparation method according to claim 1, is characterized in that range of reaction temperature 50 ~ 130 DEG C; 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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| CN103304736B true CN103304736B (en) | 2015-09-23 |
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Families Citing this family (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 |
| CN109160974B (en) * | 2018-07-27 | 2020-12-15 | 天津安浩生物科技有限公司 | Aqueous phase preparation method of maleic anhydride-conjugated diene copolymer |
| CN111484579B (en) * | 2020-04-16 | 2021-11-12 | 陕西科技大学 | High-temperature soluble bridge plug and preparation method 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 |
| 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 |
| 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 |
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 |
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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 |
|---|
| IBMA树脂的合成与表征;戚银城等;《高分子材料科学与工程》;19920331(第2期);38-43页 * |
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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. |