CN1417189A - Production process of itaconic anhydride - Google Patents
Production process of itaconic anhydride Download PDFInfo
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- CN1417189A CN1417189A CN 01135103 CN01135103A CN1417189A CN 1417189 A CN1417189 A CN 1417189A CN 01135103 CN01135103 CN 01135103 CN 01135103 A CN01135103 A CN 01135103A CN 1417189 A CN1417189 A CN 1417189A
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Abstract
The present invention relates to a production process of itaconic anhydride and belongs to the field of preparing carboxylic anhydride from carboxylic acid. It is characterized by that itaconic acid, dewatering agent and catalyst in a molar ratio of 1 to 0.95-1.5 to 0-0.15 are reacted through stirring for 0.5-6 hr at 40-85 deg.c. The dewatering agent may be selected from acetyl chloride, cis-butenedioic anhydride and acetic anhydride; and the catalyst may be selected from zinc acetate, potassium acetate and sodium acetate. The process of the present invention is one itaconic anhydride producing process capable of being used in industry and the product has melting point of 67-69 deg.c and content not less than 98%.
Description
Affiliated technical field
The invention belongs to from carboxylic acid and prepare carboxylic acid anhydride category, particularly production process of itaconic anhydride.
Background technology
It is reported, and itaconic anhydride (Itaconic, anhydride), chemical name is an itaconic anhydride, outward appearance is the rice white crystalline powder, has slight acetate smell, and is solvable in 35 ℃ of following butylacetates, fusing point 68-72 ℃, purity 〉=97%.
The domestic health acid anhydrides production report of having no clothes at present.
Not retrieved production process of itaconic anhydride, and only had 95101672.5 to mention in its PKa value to 4-10, is that organic acid-alkali type catalyzer exists heating methylene-succinic acid down to small part, prepares the method for citraconic anhydride.
Summary of the invention
The purpose of this invention is to provide a kind of industrialized production process of itaconic anhydride.
Technical scheme of the present invention is: a kind of production process of itaconic anhydride, it is characterized in that methylene-succinic acid and dewatering agent, catalyzer, by mole ratio be: methylene-succinic acid: dewatering agent: catalyzer=1: 0.95～1.5: 0～0.15, at 40～85 ℃, react 0.5～6h under stirring.
Its dewatering agent can be selected from Acetyl Chloride 98Min., MALEIC ANHYDRIDE or acetic anhydride; Its catalyzer can be selected from zinc acetate, Potassium ethanoate or sodium-acetate.
The effect that the present invention obtains is:
Obtained a kind ofly can be applied to industrialized itaconic anhydride production method, 67～69 ℃ of finished product fusing points, content 〉=98%.
Embodiment
Embodiment one is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), Acetyl Chloride 98Min. 7.477kg (content 99.1%, pure 95mole), zinc acetate 1.821kg (content 99.5%, pure 15mole), insert in the retort, in 40～45 ℃, reaction 4h, clarifying to reaction solution is reaction end, cooling, crystallization, centrifugal, dry, itaconic anhydride must be measured 7.447kg, content 98.5% (esterification process mensuration), yield 65.5%, 67～69 ℃ of finished product fusing points.
Embodiment two is methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), Acetyl Chloride 98Min. 11.81kg (content 99.1%, pure 150mole), and 40～45 ℃ of reaction 6h, itaconic anhydride must be measured 6.84kg, yield 60.2%, all the other are with example one.
Embodiment three is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), Acetyl Chloride 98Min. 7.87kg (content 99.1%, pure 100mole), zinc acetate 1.214kg (content 99.5%, pure 10mole), in 40～45 ℃, reaction 3.5h, itaconic anhydride must be measured 6.97kg, yield 61.3%, all the other are with example one.
Embodiment four is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), Acetyl Chloride 98Min. 9.445kg (content 99.1%, pure 120mole), zinc acetate 0.607kg (content 99.5%, pure 5mole), in 40～45 ℃, reaction 5.5h, itaconic anhydride must be measured 6.96kg, yield 61.2%, all the other are with example one.
Embodiment five is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), Acetyl Chloride 98Min. 10.23kg (content 99.1%, pure 130mole), zinc acetate 0.364kg (content 99.5%, pure 3mole), in 40～45 ℃, reaction 4.5h, itaconic anhydride must be measured 7.24kg, yield 63.7%, all the other are with example one.
Embodiment six is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), maleic anhydride 9.451kg (content 98.5%, pure 95mole), Potassium ethanoate 1.5kg (content 98%, pure 15mole), in 60～65 ℃, reaction 0.5h, itaconic anhydride must be measured 7.40kg, content 98.5%, yield 65.1%, all the other are with example one.
Embodiment seven is methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), maleic anhydride 14.92kg (content 98.5%, pure 150mole), and 80～85 ℃ of reaction 6h, itaconic anhydride must be measured 6.69kg, yield 60.7%, all the other are with example one.
Embodiment eight is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), maleic anhydride 9.95 kg (content 99.1%, pure 100mole), Potassium ethanoate 1.0kg (content 98%, pure 10mole), in 75～80 ℃, reaction 1.5h, itaconic anhydride must be measured 6.95kg, yield 61.1%, all the other are with example one.
Embodiment nine is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), maleic anhydride 0.5kg (content 99.1%, pure 130mole), Potassium ethanoate 0.5kg (content 98%, pure 5mole), in 70～75 ℃, reaction 2h, itaconic anhydride must be measured 7.08kg, yield 62.3%, all the other are with example one.
Embodiment ten is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), maleic anhydride 11.94kg (content 98%, pure 120mole), Potassium ethanoate 0.2kg (content 98%, pure 2mole), in 75～80 ℃, reaction 2.5h, itaconic anhydride must be measured 7.16kg, yield 63.4%, all the other are with example one.
Embodiment 11 is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), aceticanhydride 9.74kg (content 99.5%, pure 95mole), sodium-acetate 2.05kg (content 60%, pure 15mole), in 50～55 ℃, reaction 0.5h, itaconic anhydride must be measured 7.47kg, content 98.5%, yield 65.7%, all the other are with example one.
Embodiment 12 is methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), aceticanhydride 12.3kg (content 99.5%, pure 120mole), and 45～50 ℃ of reaction 6h, itaconic anhydride must be measured 6.96kg, yield 61.2%, all the other are with example one.
Embodiment 13 is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), aceticanhydride 10.25kg (content 99.5%, pure 100mole), sodium-acetate 1.366kg (content 60%, pure 10mole), in 55～60 ℃, reaction 1.5h, itaconic anhydride must be measured 7.08kg, yield 62.3%, all the other are with example one.
Embodiment 14 is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), aceticanhydride 13.33kg (content 99.5%, pure 130mole), sodium-acetate 0.683kg (content 60%, pure 5mole), in 60～65 ℃, reaction 4h, itaconic anhydride must be measured 7.16kg, yield 63.0%, all the other are with example one.
Embodiment 15 is with methylene-succinic acid 13.05kg (content 99.62%, pure 100mole), aceticanhydride 15.38kg (content 99.5%, pure 150mole), sodium-acetate 0.273kg (content 60%, pure 2mole), in 65～70 ℃, reaction 5h, itaconic anhydride must be measured 7.29kg, yield 64.1%, all the other are with example one.
Claims (3)
1. a production process of itaconic anhydride is characterized in that methylene-succinic acid and dewatering agent, catalyzer, by mole ratio is: methylene-succinic acid: dewatering agent: catalyzer=1: 0.95～1.5: 0～0.15, at 40～85 ℃, react 0.5～6h under stirring.
2. according to the described production process of itaconic anhydride of claim 1, it is characterized in that dewatering agent can select from Acetyl Chloride 98Min., MALEIC ANHYDRIDE or acetic anhydride.
3. according to the described production process of itaconic anhydride of claim 1, it is characterized in that catalyzer can select from zinc acetate, Potassium ethanoate or sodium-acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01135103 CN1208302C (en) | 2001-11-08 | 2001-11-08 | Production process of itaconic anhydride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01135103 CN1208302C (en) | 2001-11-08 | 2001-11-08 | Production process of itaconic anhydride |
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| CN1417189A true CN1417189A (en) | 2003-05-14 |
| CN1208302C CN1208302C (en) | 2005-06-29 |
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| CN 01135103 Expired - Fee Related CN1208302C (en) | 2001-11-08 | 2001-11-08 | Production process of itaconic anhydride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107540441A (en) * | 2017-07-20 | 2018-01-05 | 青岛琅琊台集团股份有限公司 | A kind of solid phosphorus efficiency bio-feritlizer of fixed nitrogen that crop yield is improved using itaconic acid |
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2001
- 2001-11-08 CN CN 01135103 patent/CN1208302C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107540441A (en) * | 2017-07-20 | 2018-01-05 | 青岛琅琊台集团股份有限公司 | A kind of solid phosphorus efficiency bio-feritlizer of fixed nitrogen that crop yield is improved using itaconic acid |
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| CN1208302C (en) | 2005-06-29 |
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