CN114560752A - Synthetic method of 2-methallyl alcohol - Google Patents
Synthetic method of 2-methallyl alcohol Download PDFInfo
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- CN114560752A CN114560752A CN202210176340.4A CN202210176340A CN114560752A CN 114560752 A CN114560752 A CN 114560752A CN 202210176340 A CN202210176340 A CN 202210176340A CN 114560752 A CN114560752 A CN 114560752A
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- C07—ORGANIC CHEMISTRY
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/09—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis
- C07C29/12—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of mineral acids
- C07C29/124—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by hydrolysis of esters of mineral acids of halides
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
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- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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Abstract
The invention provides a method for synthesizing 2-methallyl alcohol, which comprises the steps of heating a sodium acetate solution and 2-methallyl chloride under an alkaline condition for reaction, separating sodium acetate and sodium chloride from a water phase of a mixture obtained after the reaction is finished, and recycling the separated sodium acetate to the heating reaction process; and (3) separating and purifying the 2-methallyl alcohol, the sodium acetate and other components in the organic phase of the mixture after the reaction is finished, and recycling the separated sodium acetate to the heating reaction process. In the synthetic method, the esterification reaction and the saponification reaction are synchronously completed, a phase transfer catalyst is not needed in the reaction process, the reaction liquid is easy to layer, the technological process is simple, the operation is convenient, the reaction selectivity is high, and the byproducts are few; and the sodium acetate solution and the water are completely reused without additional supplement, thereby realizing the recycling.
Description
Technical Field
The invention belongs to the technical field of synthesis of organic chemical products, and particularly relates to a synthesis method of 2-methallyl alcohol.
Background
2-methylallyl alcohol, also known as 2-methyl-2-propen-1-ol, 3-hydroxy-2-methylpropylene, or isobutenol, of the formula CH2C(CH3)CH2OH, molecular weight 72.11, boiling point 113-. 2-methyl allyl alcohol is an important fine chemical raw material, can be used in the fields of medicines, pesticides, spices, resins, polycarboxylic acid water reducing agents and the like, is soluble in water and organic solvents, has similar performance to allyl alcohol but lower toxicity than allyl alcohol, and can be used as a substitute of allyl alcohol in many fields.
US2072015, CN103588622A and CN101759528A all adopt direct hydrolysis of methallyl chloride with alkali, and have the main disadvantages of more etherification by-products, low alkali solution concentration and large wastewater generation amount. US2767221, CN102167657B, CN103755523A, CN103755523 and CN106824221 all adopt methallyl aldehyde or prepare methallyl alcohol by firstly oxidizing methallyl aldehyde with isobutylene and then hydrogenating and reducing, but have the disadvantages of high hydrogenation pressure, high oxidation temperature, poor catalyst hydrogenation selectivity, easy polymerization of methallyl aldehyde and the like.
CN103242139A discloses a method for preparing 2-methyl allyl alcohol by esterification hydrolysis two-step method, i.e. 2-methyl allyl alcohol carboxylate is synthesized first, then low concentration strong base is added for hydrolysis to obtain 2-methyl allyl alcohol, but this method needs phase transfer catalyst, resulting in difficult layering of reaction system, and a large amount of waste salt and waste water containing sodium acetate are generated in the reaction. Meanwhile, the organic phase after the esterification reaction is directly subjected to hydrolysis reaction, and a certain amount of methyl allyl chloride is still contained, so that 2-methyl allyl ether with slightly high relative content is generated in the hydrolysis reaction process, and the quality of the product is influenced.
CN105037097A proposes that in the presence of a phase transfer catalyst and 2-methylallyl chloride, solid sodium acetate reacts with 2-methylallyl chloride to enable the sodium acetate to fully react, reactants are simply distilled to obtain a mixture of 2-methylallyl alcohol acetate and unreacted raw materials, the mixture is rectified to obtain the unreacted raw materials and the 2-methylallyl alcohol acetate, the unreacted raw materials are used indiscriminately, the 2-methylallyl alcohol acetate is subjected to alkali liquor saponification reaction to obtain 2-methylallyl alcohol, and water is removed from a water phase to obtain the sodium acetate which can be directly used indiscriminately in the reaction. However, the esterification reaction of the process involves a phase transfer catalyst, and the product is treated and then subjected to saponification reaction, so that the two steps of reactions are completely separated, and the operation is troublesome.
CN108191604B proposes a two-step method, in which a sodium acetate solution, 2-methallyl chloride and sodium hydroxide are added into a multistage series continuous stirring reactor to react to obtain 2-methallyl alcohol, but the process is complex, the operation cost is high, and the equipment investment cost is high.
In conclusion, there is a need to develop new economical and environmentally friendly synthetic techniques for 2-methallyl alcohol to solve the various problems existing at present.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a synthetic method of 2-methallyl alcohol, which has the advantages of reasonable process, simple operation, high product selectivity and easy industrial production. The technical scheme of the invention is as follows:
a synthetic method of 2-methyl allyl alcohol, heat sodium acetate solution and 2-methyl allyl chloride under the alkaline condition to react, carry on sodium acetate and sodium chloride separation to the aqueous phase of the mixture that finishes the reaction, sodium acetate separated is recycled to the heating reaction process; and (3) separating and purifying the 2-methallyl alcohol, the sodium acetate and other components in the organic phase of the mixture after the reaction is finished, and recycling the separated sodium acetate to the heating reaction process.
Further, the control method of the heating reaction comprises the following steps: uniformly mixing a sodium acetate solution and 2-methylallyl chloride, heating, dropwise adding a sodium hydroxide solution, controlling the pH value of the reaction solution, preserving heat after dropwise adding, and then cooling and layering.
Further, in the heating reaction, the molar ratio of 2-methylallyl chloride to sodium acetate is (0.5-1.1): 1, the reaction temperature is 100-120 ℃, the reaction is a closed reaction, the pH value of the system is adjusted by adopting a sodium hydroxide solution with the mass concentration of 30%, the pH value is controlled to be 9-11, the dropping time of the sodium hydroxide solution is 6-10 hours, and the temperature is kept for 1-2 hours after the dropping.
Further, the step of separating sodium acetate and sodium chloride from the water phase of the mixture after the reaction is completed comprises the following steps: removing a trace amount of azeotrope of methallyl alcohol and water from the water phase by using a rectifying tower, collecting the produced liquid at the top of the tower for preparing a sodium hydroxide solution, carrying out multiple-effect separation on the tower bottom liquid, and then carrying out continuous centrifugal filtration and washing to obtain sodium chloride crystals and mother liquid, wherein the mother liquid is a sodium acetate solution and is applied to the reaction, the water removed in the multiple-effect separation is used for preparing the sodium hydroxide solution, and the redundant water removing sleeve is used for a link needing water in the synthetic method.
Preferably, the tower top temperature of the rectifying tower is controlled to be 92-93 ℃.
Preferably, the multi-effect separation is specifically triple-effect separation, and the control parameters are as follows: the vacuum degree is-0.060 MPa to 0.085MPa, and the first effect temperature is 105 ℃ to 115 ℃.
Further, the separation and purification of the 2-methallyl alcohol, the sodium acetate and other components in the organic phase of the mixture after the reaction is finished comprises the following steps: distilling the organic phase under reduced pressure in a distillation still to obtain a mixture of 2-methallyl alcohol and trace 2-methallyl ether, wherein the residual solid in the distillation still is mainly sodium acetate solid, and adding water for dissolving and mechanically applying until heating reaction; and (3) rectifying the mixture of the 2-methallyl alcohol and the trace 2-methallyl ether at normal pressure to remove the trace 2-methallyl ether, then removing moisture through azeotropic rectification to obtain the 2-methallyl alcohol, wherein the moisture removed in the azeotropic rectification is used for dissolving sodium acetate solid remained in the distillation kettle and is indiscriminately applied to heating reaction.
Further, the temperature of the organic phase subjected to reduced pressure distillation through a distillation kettle is 65-115 ℃, the vacuum degree of the reduced pressure distillation is-0.080 MPa to-0.090 MPa, and the time of the reduced pressure distillation is 4-9 h.
Further, the temperature of the top of the tower for removing trace 2-methylallyl ether by normal pressure rectification is controlled to be 84-86 ℃.
Further, the temperature of the top of the azeotropic distillation dehydration tower is controlled to be 92-93 ℃.
Compared with the prior art, the invention has the following outstanding advantages and positive effects:
in the synthetic method, the esterification reaction and the saponification reaction are synchronously completed, a phase transfer catalyst is not needed in the reaction process, the reaction liquid is easy to layer, the technological process is simple, the operation is convenient, the reaction selectivity is high, and the byproducts are few; and the sodium acetate solution and the water are completely reused without additional supplement, thereby realizing recycling.
Detailed Description
In the description of the present invention, it is to be noted that those whose specific conditions are not specified in the examples are carried out according to the conventional conditions or the conditions recommended by the manufacturers. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
The present invention will be described in further detail with reference to specific embodiments thereof to assist those skilled in the art in providing a more complete, accurate and thorough understanding of the inventive concept and aspects thereof, and the scope of the present invention includes, but is not limited to, the following examples, and any modifications in the details and form of the technical aspects thereof that fall within the spirit and scope of the present application are intended to be included therein.
And analyzing the organic phase of the reaction product by an Agilent gas chromatograph, using an FID detector, using an HP-5 column, and using a sample inlet temperature: 230 ℃ to 230 ℃.
Detector temperature: 230 ℃, column temperature: the initial temperature is 40 deg.C, holding for 5min, heating to 130 deg.C at 10 deg.C/min, and holding for 5 min.
Example 1
588g of 2-methylallyl chloride and 2368g of sodium acetate solution (the molar ratio of 2-methylallyl chloride to sodium acetate is 0.5:1.0) are added into a reaction kettle, the mixture is stirred and heated to 100 ℃, then 30 percent of sodium hydroxide solution is dripped into the mixture, the dripping time is 6.0h, the pressure is 0.3MPa at most, the mixture is kept for reaction for 1.5h, the pH value is controlled at 9.0, and after the reaction is finished, the mixture is kept stand and layered. Transferring the material to a distillation kettle by the upper organic phase, wherein the vacuum degree of the distillation organic phase is-0.080 MPa, the temperature of the top of the distillation kettle for removing the 2-methyl allyl ether by normal pressure distillation is 84.5 ℃, the temperature of the top of the distillation kettle for azeotropic distillation and dehydration is 92.0 ℃, and the content of the obtained 2-methyl allyl alcohol is 99.93%. The temperature of the top of the aqueous phase rectifying tower is 92.3 ℃; the vacuum degree of the three-effect separation is-0.060 MPa, the one-effect temperature is 113 ℃, the content of the by-product sodium chloride obtained after the multi-effect separation and washing is more than 97.5 percent, and the centrifugal mother liquor is mechanically applied to the reaction process.
Example 2
In a reaction kettle, 588g of 2-methylallyl chloride and 2190g of sodium acetate solution (the molar ratio of 2-methylallyl chloride to sodium acetate is 0.6:1.0) are added, stirred and heated to 105 ℃, then 30 percent of sodium hydroxide solution is added dropwise for 7.0h, the pressure is 0.3MPa at most, the temperature is kept for reaction for 1.5h, the pH value is controlled at 9.5, and after the reaction is finished, standing and layering are carried out. Transferring the material to a distillation kettle by the upper organic phase, wherein the vacuum degree of the distillation organic phase is-0.080 MPa, the temperature of the top of the distillation kettle for removing the 2-methyl allyl ether by normal pressure distillation is 84.5 ℃, the temperature of the top of the distillation kettle for azeotropic distillation and dehydration is 92.2 ℃, and the content of the obtained 2-methyl allyl alcohol is 99.90%. The temperature of the top of the aqueous phase rectifying tower is 92.5 ℃; the vacuum degree of the three-effect separation is-0.065 MPa, the one-effect temperature is 111 ℃, the content of the by-product sodium chloride obtained after the multi-effect separation and washing is more than 97.4 percent, and the centrifugal mother liquor is mechanically applied to the reaction process.
Example 3
In a reaction kettle, 588g of 2-methylallyl chloride and 2063g of sodium acetate solution (the molar ratio of 2-methylallyl chloride to sodium acetate is 0.7:1.0) are added, stirred and heated to 110 ℃, then 30 percent of sodium hydroxide solution is added dropwise for 7.5h, the pressure is 0.3MPa at most, the temperature is kept for reaction for 1.5h, the pH is controlled at 9.5, and after the reaction is finished, standing and layering are carried out. Transferring the material to a distillation kettle by the upper organic phase, wherein the vacuum degree of the distillation organic phase is-0.080 MPa, the temperature of the top of the distillation kettle for removing the 2-methyl allyl ether by normal pressure distillation is 84.5 ℃, the temperature of the top of the distillation kettle for azeotropic distillation and dehydration is 92.4 ℃, and the content of the obtained 2-methyl allyl alcohol is 99.88%. The temperature of the top of the aqueous phase rectifying tower is 92.5 ℃; the vacuum degree of the three-effect separation is-0.068 MPa, the one-effect temperature is 110 ℃, the content of the by-product sodium chloride obtained after the multi-effect separation and washing is more than 97.6%, and the centrifugal mother liquor is mechanically applied to the reaction process.
Example 4
In a reaction kettle, 588g of 2-methylallyl chloride and 1968g of sodium acetate solution (the molar ratio of 2-methylallyl chloride to sodium acetate is 0.8:1.0) are added, stirred and heated to 110 ℃, then 30 percent of sodium hydroxide solution is added dropwise for 8.0h, the pressure is 0.3MPa at most, the temperature is kept for reaction for 1.5h, the pH is controlled at 10.0, and after the reaction is finished, standing and layering are carried out. Transferring the material to a distillation kettle by the upper organic phase, wherein the vacuum degree of the distillation organic phase is-0.080 MPa, the tower top temperature for removing the 2-methyl allyl ether by normal pressure distillation is 85.0 ℃, the tower top temperature for azeotropic distillation dehydration is 92.6 ℃, and the content of the obtained 2-methyl allyl alcohol is 99.87%. The temperature of the top of the water phase rectifying tower is 92.4 ℃; the vacuum degree of the three-effect separation is-0.070 MPa, the one-effect temperature is 110 ℃, the content of the by-product sodium chloride obtained after the multi-effect separation and the washing is more than 97.6 percent, and the centrifugal mother liquor is mechanically applied to the reaction process.
Example 5
In a reaction kettle, 588g of 2-methylallyl chloride and 1895g of sodium acetate solution (the molar ratio of 2-methylallyl chloride to sodium acetate is 0.9:1.0) are added, stirred and heated to 110 ℃, then 30 percent of sodium hydroxide solution is added dropwise for 8.5h, the pressure is 0.3MPa at most, the temperature is kept for reaction for 1.0h, the pH value is controlled at 10.0, and after the reaction is finished, standing and layering are carried out. Transferring the material to a distillation kettle by the upper organic phase, wherein the vacuum degree of the distillation organic phase is-0.080 MPa, the temperature of the top of the tower for removing the 2-methyl allyl ether by atmospheric distillation is 85.0 ℃, the temperature of the top of the tower for azeotropic distillation dehydration is 92.4 ℃, and the content of the obtained 2-methyl allyl alcohol is 99.85 percent. The temperature of the top of the aqueous phase rectifying tower is 92.6 ℃; the vacuum degree of the three-effect separation is-0.075 MPa, the one-effect temperature is 108 ℃, the content of the byproduct sodium chloride obtained after the multi-effect separation and washing is more than 97.4 percent, and the centrifugal mother liquor is mechanically applied to the reaction process.
Example 6
Adding 588g of 2-methylallyl chloride and 1835g of sodium acetate solution (the molar ratio of 2-methylallyl chloride to sodium acetate is 1.0:1.0), stirring and heating to 115 ℃, then beginning to dropwise add 30% of sodium hydroxide solution for 9.0h, keeping the pressure at the highest 0.3MPa for reaction for 1.0h, controlling the pH value at 10.5, and standing for layering after the reaction is finished. Transferring the material to a distillation kettle by the upper organic phase, wherein the vacuum degree of the distillation organic phase is-0.080 MPa, the temperature of the top of the tower for removing the 2-methyl allyl ether by atmospheric distillation is 85.5 ℃, the temperature of the top of the tower for azeotropic distillation dehydration is 92.6 ℃, and the content of the obtained 2-methyl allyl alcohol is 99.89%. The temperature of the top of the aqueous phase rectifying tower is 92.6 ℃; the vacuum degree of the three-effect separation is-0.080 MPa, the one-effect temperature is 107 ℃, the content of the byproduct sodium chloride obtained after the multi-effect separation and washing is more than 97.7 percent, and the centrifugal mother liquor is mechanically applied to the reaction process.
Example 7
Adding 588g of 2-methylallyl chloride and 1787g of sodium acetate solution (the molar ratio of the 2-methylallyl chloride to the sodium acetate is 1.1:1.0), stirring and heating to 115 ℃, then beginning to dropwise add 30% of sodium hydroxide solution for 10.0h, keeping the pressure at the highest 0.3MPa for reaction for 1.0h, controlling the pH value to be 11.0, and standing and layering after the reaction is finished. Transferring the material to a distillation kettle by the upper organic phase, wherein the vacuum degree of the organic phase is-0.085 MPa, the temperature of the top of the distillation kettle for removing the 2-methyl allyl ether by atmospheric distillation is 86.0 ℃, the temperature of the top of the azeotropic distillation dehydration kettle is 92.5 ℃, and the content of the obtained 2-methyl allyl alcohol is 99.84%. The temperature of the top of the aqueous phase rectifying tower is 92.5 ℃; the vacuum degree of the three-effect separation is-0.085 MPa, the one-effect temperature is 105 ℃, the content of the by-product sodium chloride obtained after the multi-effect separation and washing is more than 97.4 percent, and the centrifugal mother liquor is mechanically applied to the reaction process.
In summary, the synthesis method of the present invention has the following technical advantages:
1. the esterification reaction and the saponification reaction are synchronously completed, a phase transfer catalyst is not needed in the reaction process, the reaction liquid is easy to layer, the technological process is simple, the operation is convenient, the reaction selectivity is high, and the byproducts are few;
2. and continuously rectifying the water phase to remove residual organic matters, and carrying out three-effect separation and washing to obtain a by-product sodium chloride with the content of more than or equal to 97.0%.
3. Distilling the organic phase, removing trace 2-methallyl ether by normal pressure rectification, and then performing azeotropic rectification dehydration to obtain a product, namely 2-methallyl alcohol with high purity of over 99.8 percent;
4. the sodium acetate solution and the water are completely reused without additional supplement, thereby realizing recycling.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method for synthesizing 2-methallyl alcohol is characterized by comprising the following steps: heating sodium acetate solution and 2-methyl allyl chloride to react under alkaline condition, separating sodium acetate and sodium chloride from water phase of the mixture after reaction, and recycling the separated sodium acetate to the heating reaction process; and (3) separating and purifying the 2-methallyl alcohol, the sodium acetate and other components in the organic phase of the mixture after the reaction is finished, and recycling the separated sodium acetate to the heating reaction process.
2. The method of synthesizing 2-methallyl alcohol according to claim 1, wherein: the control method of the heating reaction comprises the following steps: uniformly mixing a sodium acetate solution and 2-methylallyl chloride, heating, dropwise adding a sodium hydroxide solution, controlling the pH value of the reaction solution, preserving heat after dropwise adding, and then cooling and layering.
3. The method of synthesizing 2-methallyl alcohol according to claim 2, wherein: in the heating reaction, the molar ratio of 2-methylallyl chloride to sodium acetate is (0.5-1.1): 1, the reaction temperature is 100-120 ℃, the reaction is a closed reaction, the pH value of the system is adjusted by adopting a sodium hydroxide solution with the mass concentration of 30%, the pH value is controlled to be 9-11, the dropping time of the sodium hydroxide solution is 6-10 hours, and the temperature is kept for 1-2 hours after the dropping.
4. The method of synthesizing 2-methallyl alcohol according to claim 1, wherein: the method for separating the sodium acetate and the sodium chloride from the water phase of the mixture after the reaction is completed comprises the following steps: removing a trace amount of azeotrope of methallyl alcohol and water from the water phase by using a rectifying tower, collecting the produced liquid at the top of the tower for preparing a sodium hydroxide solution, carrying out multiple-effect separation on the tower bottom liquid, and then carrying out continuous centrifugal filtration and washing to obtain sodium chloride crystals and mother liquid, wherein the mother liquid is a sodium acetate solution and is applied to the reaction, the water removed in the multiple-effect separation is used for preparing the sodium hydroxide solution, and the redundant water removing sleeve is used for a link needing water in the synthetic method.
5. The method of synthesizing 2-methallyl alcohol according to claim 4, wherein: the top temperature of the rectifying tower is controlled to be 92-93 ℃.
6. The method of synthesizing 2-methallyl alcohol according to claim 4, wherein: the multi-effect separation is specifically triple-effect separation, and the control parameters are as follows: the vacuum degree is-0.060 MPa to 0.085MPa, and the first effect temperature is 105 ℃ to 115 ℃.
7. The method of synthesizing 2-methallyl alcohol according to claim 1, wherein: the separation and purification of the 2-methallyl alcohol, the sodium acetate and other components in the organic phase of the mixture after the reaction is finished comprises the following steps: distilling the organic phase under reduced pressure in a distillation still to obtain a mixture of 2-methallyl alcohol and trace 2-methallyl ether, wherein the residual solid in the distillation still is mainly sodium acetate solid, and adding water for dissolving and mechanically applying until heating reaction; and (3) rectifying the mixture of the 2-methallyl alcohol and the trace 2-methallyl ether at normal pressure to remove the trace 2-methallyl ether, then removing moisture through azeotropic rectification to obtain the 2-methallyl alcohol, wherein the moisture removed in the azeotropic rectification is used for dissolving sodium acetate solid remained in the distillation kettle and is indiscriminately applied to heating reaction.
8. The method of synthesizing 2-methallyl alcohol of claim 7 wherein: the temperature of the organic phase subjected to reduced pressure distillation in a distillation kettle is 65-115 ℃, the vacuum degree of the reduced pressure distillation is-0.080 MPa-0.090 MPa, and the time of the reduced pressure distillation is 4-9 h.
9. The method of synthesizing 2-methallyl alcohol of claim 7 wherein: the temperature of the top of the tower for removing trace 2-methyl allyl ether by normal pressure rectification is controlled to be 84-86 ℃.
10. The method of synthesizing 2-methallyl alcohol of claim 7 wherein: the temperature of the top of the azeotropic distillation dehydration tower is controlled to be 92-93 ℃.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759528A (en) * | 2010-01-12 | 2010-06-30 | 宁波尖锋紫星生物科技有限公司 | Synthesizing method of 2-methallyl alcohol |
| CN107652163A (en) * | 2017-09-27 | 2018-02-02 | 荆楚理工学院 | A kind of high-purity methylallyl alcohol production method |
| CN108191604A (en) * | 2017-12-22 | 2018-06-22 | 浙江大学 | A kind of continuous method for preparing 2- methallyl alcohols |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759528A (en) * | 2010-01-12 | 2010-06-30 | 宁波尖锋紫星生物科技有限公司 | Synthesizing method of 2-methallyl alcohol |
| CN107652163A (en) * | 2017-09-27 | 2018-02-02 | 荆楚理工学院 | A kind of high-purity methylallyl alcohol production method |
| CN108191604A (en) * | 2017-12-22 | 2018-06-22 | 浙江大学 | A kind of continuous method for preparing 2- methallyl alcohols |
Non-Patent Citations (4)
| Title |
|---|
| 王斌: "2-甲基烯丙基氯的水解与酯化反应动力学研究" * |
| 王涛: "酯化水解两步"一锅法"合成2-甲基烯丙醇" * |
| 陈志荣: "2-甲基烯丙基氯水解动力学研究" * |
| 韩微微: "2-甲基烯丙醇生产技术研究进展及应用" * |
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