CN104016852A - Novel production process of fumaric acid with low color number and high purity - Google Patents

Novel production process of fumaric acid with low color number and high purity Download PDF

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Publication number
CN104016852A
CN104016852A CN201410051620.8A CN201410051620A CN104016852A CN 104016852 A CN104016852 A CN 104016852A CN 201410051620 A CN201410051620 A CN 201410051620A CN 104016852 A CN104016852 A CN 104016852A
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CN
China
Prior art keywords
fumaric acid
suction filtration
carrying
high purity
filtrate
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Pending
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CN201410051620.8A
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Chinese (zh)
Inventor
奚桢浩
赵玲
李双成
蒋杰
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East China University of Science and Technology
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East China University of Science and Technology
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Priority to CN201410051620.8A priority Critical patent/CN104016852A/en
Publication of CN104016852A publication Critical patent/CN104016852A/en
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
    • C07C51/353—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by isomerisation; by change of size of the carbon skeleton
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to an application of a novel production process of a fumaric acid with a low color number and high purity, and in particular relates to a novel production process for preparing the fumaric acid by sequentially carrying out an isomerization reaction, adsorption decoloration and secondary crystallization by taking acid water absorbed by a tail gas during an oxidation reaction of benzene anhydride as a raw material. The process comprises the following steps: a, adding a maleic acid water solution of a benzene anhydride production device into a reaction device and carrying out the isomerization reaction at a low temperature by adding a catalyst; b, sending an isomerized product into a first crystallization device and carrying out suction filtration after crystallization; c, sending a solid product obtained in the suction filtration manner into a decoloration device, adding a dissolving liquid and a decoloring agent for decoloration and then carrying out the suction filtration while being hot; and d, sending a filtrate obtained in the step c into a second crystallization device and carrying out solid-liquid separation and drying on a crystallized product so as to obtain the fumaric acid with the low color number and the high purity. According to the process, the produced fumaric acid is pure white and glossy in appearance and high in purity. Thus, the fumaric acid can serve as an industrial raw material as well as a food additive.

Description

Low look high purity fumaric acid new process of production
Technical field
The present invention relates to a kind of application of low look high purity fumaric acid new process of production, the benzene anhydride oxidized reaction end gas of particularly take absorbs sour water and prepares the new process of production of fumaric acid as raw material.
Background technology
Fumaric acid, claims again FUMARIC ACID TECH GRADE, normally by Isomerization of Maleic Acid, is formed.Fumaric acid is mainly for the production of fine chemicals intermediates such as unsaturated polyester resin, non-toxic plasticizer, vinyl acetate latex and optical bleaching agents, in medicine industry for the production of toxicide dimercaptosuccinic acid, in food service industry, as acidic flavoring agent, be also used as the intermediate of synthetic resins, mordant.
Industrial have several different methods to produce fumaric acid, its main source is, under catalyzer exists, benzene (or butylene) oxidation is generated to maleic acid (or MALEIC ANHYDRIDE), after absorbing, water decolours, add that catalyzer thiocarbamide is different carries out isomerization reaction, drying finally obtains fumaric acid finished product again.Utilize the method to produce the fumaric acid product appearance sallow obtaining, interior quality is poor, can not be for medicine and food service industry.
Summary of the invention
According to deficiency of the prior art, target of the present invention is to provide production technique that a kind of fumaric acid is new to improve the quality of fumaric acid product.
Fumaric acid production technique of the present invention comprises the following steps:
A. the maleic acid aqueous solution of PA Plant is joined to reaction unit, add catalyzer to carry out isomerization reaction, isomerisation temperature keeps 50 ℃～100 ℃, 0.5～2.0 hour reaction times; The first crystallization apparatus is delivered to reactant in described reaction to terminal afterwards.
B. in the first crystallization apparatus, to the fumaric acid aqueous solution crystallisation by cooling changing into, be cooled to sour water temperature and be 20～50 ℃ by suction filtration, isolate fumaric acid solid phase prod.
C. suction filtration gained solid fumaric acid is delivered to decoloration device, add steps d gained filtrate dissolved solids fumaric acid, under whipped state, add discoloring agent to decolour, bleaching temperature keeps 50 ℃～100 ℃, and suction filtration while hot decoloured after 0.5～2.0 hour; Filtrate is delivered to the second crystallization apparatus.
D. in the second crystallization apparatus, to previous step gained filtrate crystallisation by cooling, being cooled to sour water temperature is to carry out suction filtration after 30～60 ℃, and gained filtrate is as step c dissolved solids fumaric acid, and gained solid matter can low look high purity fumaric acid finished product after vacuum drying oven is dry.
Advantage applies of the present invention exists:
1, due to adopt first carry out isomerization reaction after adsorption bleaching carry out again the technique of secondary crystal, overcome the inefficient defect of traditional technology decolorizing and refining, the fumaric acid outward appearance that technique of the present invention obtains is pure white glossy, purity is high, compare fumaric acid L value with traditional technology and bring up to 95～99 by 80～85, purity brings up to 99.5%～99.9% by 98%～99%.
2, steps d gained of the present invention is dissolved with the filtrate cycle utilization of fumaric acid, compares fumaric acid yield bring up to 90%～95% from 80%～85% with traditional technology, and discharge of wastewater reduces greatly.
3, vacuum drying oven of the present invention, is a kind of dry equipment that carries out under negative pressure, and it utilizes the vacuum pump dehumidifier of bleeding, and working spaces, in vacuum state, makes fumaric acid in conjunction with the boiling point lowering of water, and the drying rate of material is accelerated greatly; Application vacuum drier can reduce drying temperature, prevents fumaric acid surface coking, guarantees product quality.
Embodiment
Get 2～2000 kilograms of the aqueous acids of PA Plant, 10～10000 grams of catalyzer, join (isomerization unit useful volume is 5～5000 liters) in isomerization unit, mixing speed keeps per minute 50～100 to turn, isomerisation temperature remains on 70 ℃～80 ℃, in 0.5～2.0 hour reaction times, to reaction end, deliver to the first crystallization apparatus (crystallization apparatus useful volume is 5～5000 liters).
In the first crystallization apparatus, after being cooled to 20～50 ℃, aqueous acid carries out suction filtration, and gained solid is delivered to decoloration device (decoloration device useful volume is 5～5000 liters).
Get 2～2000 kilogram of second crystallization apparatus gained filtrate, 10～10000 grams of discoloring agents join decoloration device, mixing speed keeps per minute 50～100 to turn, bleaching temperature keeps 60 ℃～80 ℃, bleaching time 0.5～1.0 hour, to after the terminal that decolours while hot suction filtration remove gac.Recycle after filter cake gac drying desorption, filtrate is delivered to the second crystallization apparatus (the second crystallization apparatus useful volume is 5～5000 liters).
In the second crystallization apparatus, after being cooled to 20～50 ℃, aqueous acid carries out suction filtration, and filtrate cycle is to decoloration device as lysate, and gained solid matter gained fumaric acid finished product L value after Vacuumdrier is dry is 97～99, and purity is 99.8%～99.9%.

Claims (9)

1. low look high purity fumaric acid new process of production, is characterized in that:
A. under catalyzer existence condition, the maleic acid aqueous solution from PA Plant is carried out to low temperature isomerization reaction;
B. isomerization reaction product is delivered to the first crystallization apparatus, and in the first crystallization apparatus, to the fumaric acid aqueous solution crystallisation by cooling changing into, suction filtration is isolated fumaric acid solid phase prod;
C. the solid fumaric acid after suction filtration is proceeded to decoloration device, add steps d gained filtrate dissolved solids fumaric acid, under whipped state, add discoloring agent to decolour, suction filtration while hot after decolouring, filtrate is delivered to the second crystallization apparatus;
D. in the second crystallization apparatus, to filtrate crystallisation by cooling, suction filtration is isolated fumaric acid solid phase prod, and filtrate, as step c fumaric acid lysate, had been both low look high purity fumaric acid finished product after gained solid matter drying equipment is dry.
2. according to claim 1, the catalyzer that step a adopts comprises aluminum chloride-hydrogenchloride, boron fluoride-hydrogen fluoride, thiocarbamide, ZSM-5 molecular sieve.
3. according to claim 1, step a isomerization reaction temperature is 50 ℃～100 ℃, preferably 60 ℃～80 ℃, and 0.5～2.0 hour reaction times.
4. according to claim 1, step a crystallisation by cooling terminal temperature is 20 ℃～50 ℃.
5. according to claim 1, the discoloring agent that step c adopts comprises aluminium iron polychloride, gac, reactive resin, atlapulgite, active sand and combination thereof.
6. according to claim 1, step c bleaching temperature is 50 ℃～100 ℃, preferably 50 ℃～80 ℃, and bleaching time 0.5～2.0 hour.
7. according to claim 1, steps d gained filtrate cycle to step c as solid fumaric acid lysate.
8. according to claim 1, steps d crystallisation by cooling terminal temperature is 30 ℃～60 ℃.
9. the drying plant that according to claim 1, steps d adopts is vacuum drying oven.
CN201410051620.8A 2014-02-17 2014-02-17 Novel production process of fumaric acid with low color number and high purity Pending CN104016852A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108484384A (en) * 2018-02-11 2018-09-04 常熟联邦化工股份有限公司 The technique for preparing fumaric acid using maleic acid waste water
CN111925287A (en) * 2020-08-14 2020-11-13 大连龙想催化化学股份有限公司 Device and method for producing fumaric acid by taking pyromellitic dianhydride tail gas washing liquid as raw material
CN112724009A (en) * 2019-10-14 2021-04-30 中国石油化工股份有限公司 Method for producing fumaric acid from maleic anhydride wastewater
CN115572225A (en) * 2022-08-29 2023-01-06 福建福瑞明德药业有限公司 Preparation method of sodium stearyl fumarate

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101024608A (en) * 2007-03-15 2007-08-29 山东宏信化工股份有限公司 Process for preparing fumaric acid by spraying acid water to benzene anhydride oxidized tail gas
CN101781188A (en) * 2010-02-26 2010-07-21 镇江市联港化学科技有限公司 Fumaric acid producing method
CN102086148A (en) * 2009-12-08 2011-06-08 天津德昊超微新材料有限公司 Recycling technique of fumaric acid waste liquid
CN103204772A (en) * 2012-01-17 2013-07-17 新疆金源石油化工有限公司 Method for producing fumaric acid by maleic anhydride waste water
CN103204773A (en) * 2013-04-18 2013-07-17 湘潭大学 Method for preparing fumaric acid through cis-trans isomerization of maleic acid

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101024608A (en) * 2007-03-15 2007-08-29 山东宏信化工股份有限公司 Process for preparing fumaric acid by spraying acid water to benzene anhydride oxidized tail gas
CN102086148A (en) * 2009-12-08 2011-06-08 天津德昊超微新材料有限公司 Recycling technique of fumaric acid waste liquid
CN101781188A (en) * 2010-02-26 2010-07-21 镇江市联港化学科技有限公司 Fumaric acid producing method
CN103204772A (en) * 2012-01-17 2013-07-17 新疆金源石油化工有限公司 Method for producing fumaric acid by maleic anhydride waste water
CN103204773A (en) * 2013-04-18 2013-07-17 湘潭大学 Method for preparing fumaric acid through cis-trans isomerization of maleic acid

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
郝立勇等: "自生产苯酐废水中提取富马酸工艺技术", 《山东化工》, vol. 32, no. 1, 31 December 2003 (2003-12-31), pages 6 - 7 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108484384A (en) * 2018-02-11 2018-09-04 常熟联邦化工股份有限公司 The technique for preparing fumaric acid using maleic acid waste water
CN112724009A (en) * 2019-10-14 2021-04-30 中国石油化工股份有限公司 Method for producing fumaric acid from maleic anhydride wastewater
CN112724009B (en) * 2019-10-14 2022-11-25 中国石油化工股份有限公司 Method for producing fumaric acid from maleic anhydride wastewater
CN111925287A (en) * 2020-08-14 2020-11-13 大连龙想催化化学股份有限公司 Device and method for producing fumaric acid by taking pyromellitic dianhydride tail gas washing liquid as raw material
CN115572225A (en) * 2022-08-29 2023-01-06 福建福瑞明德药业有限公司 Preparation method of sodium stearyl fumarate

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Application publication date: 20140903