CN101811957A - Preparation method of 2,2-dimethylbenzanthracene - Google Patents
Preparation method of 2,2-dimethylbenzanthracene Download PDFInfo
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- CN101811957A CN101811957A CN201010147436A CN201010147436A CN101811957A CN 101811957 A CN101811957 A CN 101811957A CN 201010147436 A CN201010147436 A CN 201010147436A CN 201010147436 A CN201010147436 A CN 201010147436A CN 101811957 A CN101811957 A CN 101811957A
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- dimethylolpropionic acid
- butyraldehyde
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Abstract
The invention discloses a preparation method of 2,2-dimethylbenzanthracene, which comprises the steps of: adding a certain quantity of formaldehyde, butyraldehyde and a catalyst to a flask; reacting for 2 to 10 hours at 20 DEG C to 50 DEG C; filtering out the catalyst; evaporating out the unreacted formaldehyde and the butyraldehyde; reducing the temperature to normal temperature; adding a certain quantity of water; heating to 40 DEG C to 80 DEG C; adding a certain quantity of hydrogen peroxide; reacting for 2 to 5 hours; evaporating out unreacted matter; and cooling and carrying out suction filtration for obtaining white crystals, namely 2,2-dimethylbenzanthracene. The invention has the advantages of high yield, fewer three wastes and simple operation.
Description
Technical field
The present invention relates to a kind of 2, the preparation method of 2-dimethylolpropionic acid.
Background technology
2, contain two reactive methylols in 2-dimethylolpropionic acid (DMBA) molecule with on the carbon atom that carboxyl links to each other, so it is widely used as the monomer of urethane and polyester, to introduce carboxylic group.By advancing neutralization reaction, during its energy is soluble in water with amine substance.This product can be widely used in aspects such as aqurous ployurethane, polyester, Resins, epoxy.Aspect solvability, DMBA has the unique advantage of oneself, and its fabulous solvability can be increased work efficiency greatly.Because the performance of DMBA is much better than dimethylol propionic acid (DMPA), the foreign market demand of dimethylolpropionic acid is very vigorous.
At present, 2, the synthesis technique of 2-dimethylolpropionic acid is mainly with mineral alkali (yellow soda ash, sodium hydroxide), mixed base (mixture of yellow soda ash and sodium hydroxide) or organic bases (triethylamine), has problems such as reactive poor, complex process, energy consumption height, environmental pollution are serious.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of technology simply, efficiently 2, the preparation method of 2-dimethylolpropionic acid.
For achieving the above object, the present invention realizes by the following technical solutions:
2, the preparation method of 2-dimethylolpropionic acid may further comprise the steps: add a certain amount of formaldehyde, butyraldehyde and catalyzer in flask, catalyzer is removed by filter after 2-10 hour in reaction under 20-50 ℃, steam except that behind unreacted formaldehyde and the butyraldehyde, reduce to normal temperature, add a certain amount of water, be heated to 40-80 ℃, add a certain amount of hydrogen peroxide, reacted 2-5 hour, and steamed and remove unreacted reactant, cooling back suction filtration obtains white crystal, be 2, the 2-dimethylolpropionic acid.
The 1.5-3.0 that described formaldehyde consumption is the butyraldehyde mole number doubly.
Described catalyst levels is 0.05-0.30 a times of butyraldehyde quality.
Described water consumption is 1-3 a times of butyraldehyde quality.
The 1.0-2.0 that described hydrogen peroxide consumption is the butyraldehyde mole number doubly.
Described catalyzer is activated carbon supported alkaline catalysts.
Described activated carbon supported alkaline catalysts, its preparation method is: with gac add in 30% liquid caustic soda stir 5-24 hour after, filter, after the gac oven dry, put into retort furnace at 400-600 ℃, under the nitrogen protection, activate 2-5 hour.
Beneficial effect of the present invention is: the yield height, and the three wastes are few, and are simple to operate, and side reaction is little, and is cheap and be easy to preserve.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1
The preparation of activated carbon supported alkaline catalysts:
With gac add in 30% liquid caustic soda stir 24 hours after, filter, after the gac oven dry, put into retort furnace at 600 ℃, under the nitrogen protection, activate after 5 hours, be catalyzer.
2, the preparation of 2-dimethylolpropionic acid:
In flask, add formaldehyde 45g, butyraldehyde 72g and catalyzer 3.6g, after 10 hours catalyzer is removed by filter in reaction under 50 ℃, steam except that behind unreacted formaldehyde and the butyraldehyde, reduce to normal temperature, add 72g water, be heated to 80 ℃, add the 34g hydrogen peroxide, reacted 2 hours, and steamed and remove unreacted reactant, cooling back suction filtration obtains white crystal, both be 2, the 2-dimethylolpropionic acid.
Embodiment 2
The preparation of activated carbon supported alkaline catalysts:
With gac add in 30% liquid caustic soda stir 5 hours after, filter, after the gac oven dry, put into retort furnace at 400 ℃, under the nitrogen protection, activate after 2 hours, be catalyzer.
2, the preparation of 2-dimethylolpropionic acid
In flask, add a certain amount of formaldehyde 90g, butyraldehyde 72g and catalyzer 21.6g, after 10 hours catalyzer is removed by filter in reaction under 50 ℃, steam except that behind unreacted formaldehyde and the butyraldehyde, reduce to normal temperature, add 216g water, be heated to 40 ℃, add the 68g hydrogen peroxide, reacted 5 hours, and steamed and remove unreacted reactant, cooling back suction filtration obtains white crystal, be 2, the 2-dimethylolpropionic acid.
Claims (8)
1. one kind 2, the preparation method of 2-dimethylolpropionic acid is characterized in that, in flask, add a certain amount of formaldehyde, butyraldehyde and catalyzer, after 2-10 hour catalyzer is removed by filter in reaction under 20-50 ℃, steam except that behind unreacted formaldehyde and the butyraldehyde, reduce to normal temperature, add a certain amount of water, be heated to 40-80 ℃, add a certain amount of hydrogen peroxide, reacted 2-5 hour, steam and remove unreacted reactant, cooling back suction filtration obtains white crystal, is 2, the 2-dimethylolpropionic acid.
2. described 2 according to claims 1, the preparation method of 2-dimethylolpropionic acid is characterized in that, the 1.5-3.0 that described formaldehyde consumption is the butyraldehyde mole number doubly.
3. described 2 according to claims 1, the preparation method of 2-dimethylolpropionic acid is characterized in that, described catalyst levels be the butyraldehyde quality 0.05-0.30 doubly.
4. described 2 according to claims 1, the preparation method of 2-dimethylolpropionic acid is characterized in that, described water consumption be the butyraldehyde quality 1-3 doubly.
5. described 2 according to claims 1, the preparation method of 2-dimethylolpropionic acid is characterized in that, the 1.0-2.0 that described hydrogen peroxide consumption is the butyraldehyde mole number doubly.
6. described 2 according to claims 1, the preparation method of 2-dimethylolpropionic acid is characterized in that, described catalyzer is activated carbon supported alkaline catalysts.
7. according to claims 6 described 2; the preparation method of 2-dimethylolpropionic acid; it is characterized in that; described activated carbon supported alkaline catalysts; its preparation method is: with gac add in 30% liquid caustic soda stir 5-24 hour after, filter, after the gac oven dry; put into retort furnace at 400-600 ℃, nitrogen protection is activation down.
8. described 2 according to claims 7, the preparation method of 2-dimethylolpropionic acid is characterized in that, described preparation method, and described soak time is 2-5 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010147436A CN101811957A (en) | 2010-04-06 | 2010-04-06 | Preparation method of 2,2-dimethylbenzanthracene |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010147436A CN101811957A (en) | 2010-04-06 | 2010-04-06 | Preparation method of 2,2-dimethylbenzanthracene |
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| CN101811957A true CN101811957A (en) | 2010-08-25 |
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| CN201010147436A Pending CN101811957A (en) | 2010-04-06 | 2010-04-06 | Preparation method of 2,2-dimethylbenzanthracene |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709025A (en) * | 2013-12-30 | 2014-04-09 | 万华化学集团股份有限公司 | Preparation method for 2,2-dimethylol alkanoic acid |
| CN105085241A (en) * | 2015-08-18 | 2015-11-25 | 湖州长盛化工有限公司 | Preparation method of 2,2-dimethylolbutyric acid |
| CN106563506A (en) * | 2016-11-04 | 2017-04-19 | 浙江工业大学 | Solid alkali catalyst as well as preparation and application thereof |
| CN108558652A (en) * | 2018-06-20 | 2018-09-21 | 李先明 | A method of preparing 2,2- dimethylolpropionic acids |
| CN108658752A (en) * | 2018-06-20 | 2018-10-16 | 江西吉煜新材料有限公司 | A method of preparing 2,2- dihydromethyl propionic acids |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101195567A (en) * | 2007-12-13 | 2008-06-11 | 吴江市方霞企业信息咨询有限公司 | Preparation method of dimethylolbutyric acid |
-
2010
- 2010-04-06 CN CN201010147436A patent/CN101811957A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101195567A (en) * | 2007-12-13 | 2008-06-11 | 吴江市方霞企业信息咨询有限公司 | Preparation method of dimethylolbutyric acid |
Non-Patent Citations (2)
| Title |
|---|
| 史红月等: "2,2-二羟甲基丁酸的合成", 《精细化工》, vol. 20, no. 2, 28 February 2003 (2003-02-28), pages 101 - 104 * |
| 张伟光: "2,2-二羟甲基丁酸的合成工艺研究", 《齐齐哈尔大学学报》, vol. 16, no. 4, 31 December 2000 (2000-12-31), pages 77 - 78 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709025A (en) * | 2013-12-30 | 2014-04-09 | 万华化学集团股份有限公司 | Preparation method for 2,2-dimethylol alkanoic acid |
| CN105085241A (en) * | 2015-08-18 | 2015-11-25 | 湖州长盛化工有限公司 | Preparation method of 2,2-dimethylolbutyric acid |
| CN106563506A (en) * | 2016-11-04 | 2017-04-19 | 浙江工业大学 | Solid alkali catalyst as well as preparation and application thereof |
| CN108558652A (en) * | 2018-06-20 | 2018-09-21 | 李先明 | A method of preparing 2,2- dimethylolpropionic acids |
| CN108658752A (en) * | 2018-06-20 | 2018-10-16 | 江西吉煜新材料有限公司 | A method of preparing 2,2- dihydromethyl propionic acids |
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Application publication date: 20100825 |