CN1298689C - Technique of alkaline process for producing sodium methoxide/sodium ethylate - Google Patents
Technique of alkaline process for producing sodium methoxide/sodium ethylate Download PDFInfo
- Publication number
- CN1298689C CN1298689C CNB2004100355611A CN200410035561A CN1298689C CN 1298689 C CN1298689 C CN 1298689C CN B2004100355611 A CNB2004100355611 A CN B2004100355611A CN 200410035561 A CN200410035561 A CN 200410035561A CN 1298689 C CN1298689 C CN 1298689C
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- Prior art keywords
- dehydration
- molecular sieve
- alkaline process
- technology
- sodium
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000000034 method Methods 0.000 title claims abstract description 25
- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 title claims description 14
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 title abstract description 10
- 239000002808 molecular sieve Substances 0.000 claims abstract description 33
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 claims abstract description 31
- 230000018044 dehydration Effects 0.000 claims abstract description 18
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005516 engineering process Methods 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 238000010521 absorption reaction Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 238000003795 desorption Methods 0.000 abstract description 8
- 230000001476 alcoholic effect Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 3
- 239000011734 sodium Substances 0.000 abstract description 3
- 229910052708 sodium Inorganic materials 0.000 abstract description 3
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract 1
- 239000002893 slag Substances 0.000 abstract 1
- 239000002912 waste gas Substances 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 21
- 239000007789 gas Substances 0.000 description 10
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- KIDXYAWWICJAFK-UHFFFAOYSA-N O.[Na].OC Chemical compound O.[Na].OC KIDXYAWWICJAFK-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a new technology for producing sodium methoxide/ sodium alcoholate with an alkali method, which belongs to the technical field of chemosynthesis. Superfluous sodium methoxide/ sodium alcoholate is used for reacting to sodium hydroxide, a product is produced at the bottom of a reaction vessel, and after dehydrated, evaporated ethanol steam is returned to the reaction vessel for being circularly used. The dehydration of the ethanol steam is carried out through at least two molecular sieves which are connected in parallel, and the adsorption and the desorption are alternately carried out. The adoption of the molecular sieve for dehydration makes dehydration depth high and dehydration speed fast, and shortens production period. The connection of at least two molecular sieves in parallel can make the adsorption and the desorption alternately carried out, and makes continuous automatic production realized. The operation of the new technology is simple and convenient, and the production efficiency of the new technology is high. A dilute alcoholic solution obtained through the desorption can be distilled and concentrated by a rectification device, and the concentration of the dilute alcoholic solution can reach 99.9%. Therefore, the dilute alcoholic solution can be used as a raw material for being sequentially returned for use. The technology of the present invention has no waste water discharge, no waste gas discharge, no waste slag discharge or no pollution, and has remarkable economic and social benefits.
Description
Technical field
The present invention relates to a kind of novel process of alkaline process production first/sodium ethylate, belong to chemosynthesis technical field.
Background technology
Traditional sodium method production first/sodium ethylate is by first/ethanol and sodium Metal 99.5 reaction, and sodium Metal 99.5 raw materials cost height is active big, inflammable and explosive, dangerous big.Alkaline process production then with first/ethanol and sodium hydroxide reaction, is suitable for industrial production.In the alkaline process production method, pure dehydration is crucial, and existing way is that aqueous alcohol steam is dewatered with rectificating method, and the production cycle is long, and production efficiency is low, consumes height, is not easy to realize continuous, automatic production.
Summary of the invention
The object of the present invention is to provide a kind of novel process of alkaline process production first/sodium ethylate, dehydration degree of depth height, with short production cycle, production efficiency height, continuous, the automatic production of convenient realization.
Alkaline process production first of the present invention/sodium ethylate technology, with excessive first/ethanol and sodium hydroxide reaction, the bottom output product of reactor, the pure steam that evaporates recycles through dehydration back Returning reactor, and its technical essential is that molecular sieve dehydration is adopted in pure steam dehydration.
Molecular sieve dehydration, dehydration degree of depth height, dewatering speed is fast, has shortened the production cycle, has improved production efficiency, is convenient to realize continuous, automatic production by the pipeline connection.
Insert two with molecular sieve is in parallel at least, absorption, desorb are hocketed, make continuous, automatic production become possibility.
Wherein:
Desorb can be adopted the negative pressure desorption method, and the alcohol-water mixture of absorption is extracted out, is generally undertaken by vacuum pump.Also can adopt normal pressure rare gas element desorption method, rare gas element is blown into molecular sieve discharges alcohol-water mixture, generally be temperature to be higher than 100 ℃ rare gas element, as helium, argon gas, nitrogen etc., be blown into the molecular sieve from the top of molecular sieve adsorption, desorption device, the alcohol-water mixture that adsorbs in the molecular sieve is discharged, finish desorb, realize the molecular sieve functional regeneration.
The pure steam that reactor evaporates enters molecular sieve after preferably at first passing through pressurized treatment again, improves syneresis, promotes speed of response, promotes the carrying out of reaction, further enhances productivity.
Add first/alcohol gas from the bottom of reactor, can fast reaction speed, impel reaction to carry out continuously.
First/alcohol gas after the dehydration adds from the bottom of reactor, can reduce material consumption and energy consumption, enhances productivity.
The present invention has adopted molecular sieve dehydration, dehydration degree of depth height, and dewatering speed is fast, shortened the production cycle,, absorption, desorb have been hocketed two of molecular sieve accesses in parallel at least, make continuously, automatic production becomes possibility, and is easy and simple to handle, the production efficiency height.The rare alcoholic solution that obtains through desorb can be carried dense again through rectifier unit rectifying, can be used as raw material and continue to return and come into operation.Technology three-waste free discharge of the present invention and any pollution, economic benefit and obvious social benefit.
Description of drawings
Fig. 1, one embodiment of the invention process flow diagram are example to produce the desorb of sodium methylate negative pressure.
Embodiment
The present invention is further illustrated below in conjunction with embodiment and accompanying drawing thereof.
Alkaline process of the present invention is produced sodium methylate technology, the methanol vapor that is produced by reboiler is taken and is entered in the reactor continuously with methanol gas after the dehydration and 50～80% sodium hydrate methanol solution, the aqueous methanol steam that reaction produces is pressurized to about 0.17Mpa through supercharging blower, enter from molecular sieve I bottom and to dewater, in molecular sieve I, water is absorbed (containing methyl alcohol 25% approximately) by microporous molecular sieve, obtain the methanol gas Returning reactor of content more than 99.8% from molecular sieve I top and continue to participate in reaction; When molecular sieve I absorption when saturated, switch to molecular sieve II by by-pass valve control and proceed absorption, molecular sieve I begins desorption and regeneration, and regenerative process is taken out negative with vacuum pump to molecular sieve I, water in the micropore and methyl alcohol are desorbed, thereby realize regenerating molecular sieve.When molecular sieve II absorption when saturated, switch to molecular sieve I again and adsorb, molecular sieve II begins desorption and regeneration again, periodic cycle realizes continuous production successively, and blocked operation is designed to automatization, can realize automatization control.
The dilute methanol of separating sucking-off is carried returning as raw material after dense through the rectifying of batch fractionating device and is continued to participate in reaction and use.
Basic and last same about the production technique of sodium ethylate, those skilled in the art can both understand, accepts, realize, repeat no more.
About the desorb of normal pressure rare gas element, just the top of rare gas element from molecular sieve is blown into the molecular sieve, the alcohol-water mixture that adsorbs in the molecular sieve is discharged, other also with last basic identical, similar, also no longer repeats.
Claims (7)
1, a kind of alkaline process production first/sodium ethylate technology is reacted with excessive first/ethanol and sodium hydroxide, the bottom output product of reactor, and the pure steam that evaporates recycles through dehydration back Returning reactor, it is characterized in that pure steam dehydration employing molecular sieve dehydration.
2, alkaline process production first according to claim 1/sodium ethylate technology is characterized in that two of molecular sieve accesses in parallel at least, and absorption, desorb hocket.
3, alkaline process production first according to claim 2/sodium ethylate technology is characterized in that the desorb of desorb employing negative pressure, and the alcohol-water mixture of absorption is extracted out.
4, alkaline process production first according to claim 2/sodium ethylate technology is characterized in that the desorb of desorb employing normal pressure rare gas element, rare gas element is blown into molecular sieve alcohol-water mixture is discharged.
5, alkaline process production first according to claim 1/sodium ethylate technology is characterized in that the pure steam that reactor evaporates enters molecular sieve again through after the supercharging.
6,, it is characterized in that adding first/alcohol gas from the bottom of reactor according to claim 1,2,3,4 or 5 described alkaline process production first/sodium ethylate technologies.
7, alkaline process production first according to claim 6/sodium ethylate technology, the first/alcohol gas after it is characterized in that dewatering adds from the bottom of reactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100355611A CN1298689C (en) | 2004-08-13 | 2004-08-13 | Technique of alkaline process for producing sodium methoxide/sodium ethylate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100355611A CN1298689C (en) | 2004-08-13 | 2004-08-13 | Technique of alkaline process for producing sodium methoxide/sodium ethylate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1626488A CN1626488A (en) | 2005-06-15 |
| CN1298689C true CN1298689C (en) | 2007-02-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100355611A Expired - Fee Related CN1298689C (en) | 2004-08-13 | 2004-08-13 | Technique of alkaline process for producing sodium methoxide/sodium ethylate |
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| Country | Link |
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| CN (1) | CN1298689C (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104341270A (en) * | 2013-07-30 | 2015-02-11 | 泉州恒河化工有限公司 | Sodium methoxide and dimethyl ether combined production technology |
| CN103387483B (en) * | 2013-08-14 | 2015-06-17 | 重庆紫光化工股份有限公司 | Production device and process of methanol alkali metal salts |
| CN104888494B (en) * | 2015-06-11 | 2017-01-04 | 四川九渊医药科技有限公司 | A kind of alcohol recovery system |
| CN106045813B (en) * | 2016-01-04 | 2018-09-18 | 武汉理工大学 | The method that ball-milling method prepares sodium ethoxide |
| CN105884586B (en) * | 2016-04-21 | 2019-01-22 | 赖明空 | A method and device for co-producing sodium methoxide with methanol gas phase dehydration device for producing dimethyl ether |
| CN105884578B (en) * | 2016-04-21 | 2018-11-27 | 赖明空 | A kind of method and device thereof of high temperature and pressure production sodium methoxide |
| CN109734557A (en) * | 2019-01-11 | 2019-05-10 | 盐城工业职业技术学院 | A kind of production method of sodium alkoxide |
| CN112209808A (en) * | 2020-09-15 | 2021-01-12 | 安徽金邦医药化工有限公司 | Novel process for producing sodium methoxide |
| CN115745743B (en) * | 2022-11-24 | 2024-06-18 | 河南盛宏丰化工有限公司 | Production process of liquid sodium methoxide |
| CN117550955A (en) * | 2023-11-07 | 2024-02-13 | 常州工学院 | A kind of preparation method of sodium tert-butoxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1036945A (en) * | 1988-03-29 | 1989-11-08 | 阿托化学公司 | The preparation method of fluorine-containing sodium alkoxide |
| CN1409696A (en) * | 1999-12-08 | 2003-04-09 | 巴斯福股份公司 | The preparation method of alkali metal methoxide |
-
2004
- 2004-08-13 CN CNB2004100355611A patent/CN1298689C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1036945A (en) * | 1988-03-29 | 1989-11-08 | 阿托化学公司 | The preparation method of fluorine-containing sodium alkoxide |
| CN1409696A (en) * | 1999-12-08 | 2003-04-09 | 巴斯福股份公司 | The preparation method of alkali metal methoxide |
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| Publication number | Publication date |
|---|---|
| CN1626488A (en) | 2005-06-15 |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Shandong Xinghui Chemical Co., Ltd. Assignor: Yu Zhibo Contract fulfillment period: 2008.1.1 to 2015.1.1 contract change Contract record no.: 2009370000146 Denomination of invention: Technique of alkaline process for producing sodium methoxide/sodium ethylate Granted publication date: 20070207 License type: Exclusive license Record date: 2009.7.7 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2008.1.1 TO 2015.1.1; CHANGE OF CONTRACT Name of requester: SHANDONG XINGHUI CHEMICAL INDUSTRY CO., LTD. Effective date: 20090707 |
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| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070207 Termination date: 20100813 |