CN104961631A - Methylal purifying method - Google Patents
Methylal purifying method Download PDFInfo
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- CN104961631A CN104961631A CN201510273594.8A CN201510273594A CN104961631A CN 104961631 A CN104961631 A CN 104961631A CN 201510273594 A CN201510273594 A CN 201510273594A CN 104961631 A CN104961631 A CN 104961631A
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- methylal
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/48—Preparation of compounds having groups
- C07C41/58—Separation; Purification; Stabilisation; Use of additives
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a methylal purifying method. The method comprises the following steps: adding water with the weight 0.2-3 times the weight of methylal into methylal with the mass concentration being smaller than 95%, fully and uniformly stirring, standing for 20-40min for layering, adding a drying agent to the obtained upper layer in order to dry the upper layer, stirring for 5-15min, filtering out the drying agent to obtain methylal with the mass concentration being greater than 99.5%, and dehydrating the water-containing drying agent to recycle the drying agent, wherein the absorbed water weight of the drying agent is 1-12 times the water weight of methylal. Water is added to methylal as an extractant in order to realize extraction, so the cost is low; and the purifying method also has the advantages of simplicity, mild conditions, large purifying capacity, industrial continuous production benefiting, stable and reliable mass concentration and no other impurities. Methylal is purified through rectification by using a high pressure rectification system, so the method has the advantages of low mass requirements of a raw material, high purification yield, less energy, industrial continuous production benefiting, no emission of harmful substances, and environmental protection benefiting.
Description
Technical field
The present invention relates to a kind of extraction agent to the method for methylal of purifying.
The invention still further relates to a kind of high-pressure rectification system to the method for methylal of purifying.
Background technology
The production technique of methylal is that methyl alcohol and formaldehyde react under the condition of catalyzer, then obtains methylal through rectifying.Due to methylal and methanol azeotropic, so have methyl alcohol to exist in the methylal obtained, purity is not high, and the highest mass concentration is only in being 92%.Such methylal can only be used for paint solvent and the fuel dope of poor benefit, significantly limit the Application Areas of methylal, and the methylal of high concentration has a wide range of applications.
The method of purification of current methylal adopts the mode of extraction agent high-pressure rectification and gas-liquid counter current mostly.The extraction agent that the mode of extraction agent high-pressure rectification adopts is mostly organic solvent and rectifying is complicated, extraction agent as used in Chinese patent " 200710022224.2 " is many glycol dimethyl ethers, this extraction agent not only cost is higher, and contaminative is comparatively strong, is unsuitable for a large amount of life-time service.
The mode of gas-liquid counter current, as Chinese patent " 95195524.1 " adopts polyalkylene or derivatives thereof to carry out gas-liquid counter current contact with purification methylal, this mode required equipment requires higher, and input cost is large, and complicated operation, is unsuitable for generally applying.
Therefore a kind of new technical scheme should be provided to purify to methylal, to expand its use range.
Summary of the invention
In order to overcome the technological deficiency existed in above-mentioned prior art, the object of the invention is to, providing a kind of unharmful substance to discharge, purification efficiency is high, be beneficial to environmental protection, and the method for purification of methylal simple to operate.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
A kind of method of purification of methylal, comprise the steps: in the methylal of mass concentration <90%, add water and fully stir evenly, the weight that adds water is 0.2 ~ 3 times of methylal folding hundred amounts, layering is carried out after static 20 ~ 40min, add siccative in upper strata and carry out drying, and stir 5 ~ 15 minutes, its water suction weight of the siccative added is 1 ~ 12 times of methylal weight in wet base in upper strata, filter out siccative after drying and namely obtain the methylal that mass concentration is greater than 99.5%, gained lower floor is methylal, the mixture of first alcohol and water, the lower floor of rectifying at normal temperatures and pressures mixture, reclaim methylal and methyl alcohol, or in lower floor's mixture, add formaldehyde through catalyzing and synthesizing methylal, hydrous desiccant is recyclable recycling after dehydration.
Wherein, described siccative is: molecular sieve, magnesium sulfate, aluminum oxide, barium oxide, calcium oxide, calcium chloride, sodium sulfate, calcium sulfate, silica gel any one, two or more mixture.
Have, the method comprises the steps: the methylal first adding 0.25 ~ 0.75 mass concentration <95% accounting for this system reboiler capacity in high-pressure rectification system, then nitrogen is filled with, reach after 0.1 ~ 0.8Mpa until system pressure, heat up, backflow, and collect tower top temperature and reach cut within the scope of 63.5 ~ 117.7 DEG C, again toward the methylal of additional mass concentration <95% in high-pressure rectification system while collection cut, 0.25 ~ 0.75 of this system reboiler capacity is accounted for keep this intrasystem methylal, after charging completes, stop collecting when tower top temperature reaches 63.9 ~ 118.0 DEG C, the cut collected is lowered the temperature through condenser condenses, namely mass concentration >99.5% methylal is obtained after row pressure, the mixture of to be mass concentration be 99% methyl alcohol of liquid at the bottom of the tower of gained and a small amount of methylal.
Wherein, described system pressure is 0.2 ~ 0.6Mpa, and tower top temperature is 63.7 ~ 104.7 DEG C.
Advantage of the present invention is: in methylal, add water, extracts, and extraction agent is water, and cost is low, and purifying technique is simple, mild condition, and purification amount is large, and be beneficial to industrial continuous large production, mass concentration is reliable and stable, without other impurity.Utilize the mode of high-pressure rectification system rectifying to purify to methylal, feed quality requirements is low, and purification efficiency is high, and energy requirement is few, is beneficial to industrial continuous large production, and unharmful substance discharges, and is beneficial to environmental protection.Methylal after purification has purposes very widely, and it has important application in fields such as aerosol, paint remover, refrigeration agent, makeup, clean-out system, lustering agent, pesticide solvent, coating, fuel or fuel dopes.
Embodiment
Below in conjunction with specific embodiment, further detailed description explanation is done to technical scheme of the present invention.
Embodiment 1
Toward 100kg mass concentration be 91% methylal in add 10kg water fully stirring evenly, after static 20 minutes, layering, obtain upper solution 63.5kg, in upper solution, adding 2.0kg anhydrous magnesium sulfate, (2.0kg anhydrous magnesium sulfate water regain is 2.0kg, 63.5kg upper strata water content is about 1.9kg), and stir 5 minutes, filter out siccative after drying and obtain the methylal that 60.1kg mass concentration is 99.6%, gained lower floor solution is the mixture of methylal, first alcohol and water, reclaims methylal and methyl alcohol by rectifying; Aqueous magnesium sulfate recycling after dehydration.
Embodiment 2
Toward 200kg mass concentration be 86% methylal in add 30kg water fully stirring evenly, static 30 minutes, layering, obtain upper solution 85.6kg, in upper solution, add 10kg Calcium Chloride Powder Anhydrous (10kg Calcium Chloride Powder Anhydrous water regain is that 9.7kg, 85.6kg upper solution water content is about 2.6kg), and stir 10 minutes, filter out siccative after drying and obtain the methylal that 81.1kg mass concentration is 99.7%, gained lower floor solution is the mixture of methylal, first alcohol and water, can be used for the synthesis of methylal; The reuse after dehydration of moisture calcium chloride.
Embodiment 3
Toward 500g mass concentration be 86% methylal in add 150g water fully stirring evenly, static 35 minutes, use separating funnel layering, obtain upper solution 393g, 10g molecular sieve is added in upper solution, stir 5 minutes with glass cylinder, filter out siccative and obtain the methylal that 381g mass concentration is 99.5%, gained lower floor solution 257g is the mixture of methylal, first alcohol and water; The recycling after dehydration of moisture molecular sieve.
Embodiment 4
Toward 200g mass concentration be 86% methylal in add 400g water fully stirring evenly, static 40 minutes, layering, obtain upper solution 55.6g, in upper solution, adding the mixture of 10g activated alumina and 10g sodium sulfate, (water regain of the mixture of 10g activated alumina and 10g anhydrous sodium sulphate is 20.4g, 55.6g upper solution water content is about 1.7g), and stir 15 minutes, filter out siccative after drying and obtain the methylal that 53.9g mass concentration is 99.7%, gained lower floor solution is the mixture of methylal, first alcohol and water, can be used for the synthesis of methylal; Aqueous alumina and sodium sulfate reuse after dewatering.
Embodiment 5
The methylal that 10000kg mass concentration is 90% is purified, comprise the steps: by 2000kg mass concentration be first 90% methylal squeeze in high-pressure rectification system that (the reboiler capacity of distillation system is 4m3, the volume of 2000kg methylal is 2.35m3), inflated with nitrogen, keeping system pressure is 0.2Mpa, heat up, backflow, when tower top temperature reaches 63.5 temperature, collect cut, collection cut while again toward additional mass concentration in high-pressure rectification system be the methylal of 90%, 0.25 ~ 0.75 of this system reboiler capacity is accounted for keep this intrasystem methylal, after having entered material, stop collecting when tower top temperature reaches 63.9 DEG C, cooling, row pressure, obtaining 8890kg mass concentration is the methylal of 99.7%, liquid at the bottom of tower to be 990kg mass concentration be 99% methyl alcohol.
Embodiment 6
The methylal that 20000kg mass concentration is 85% is purified, comprise the steps: by 2000kg mass concentration be first 85% methylal squeeze in high-pressure rectification system that (the reboiler capacity of distillation system is 4m3, the volume of 2000kg methylal is 1.25m3), inflated with nitrogen, keeping system pressure is 0.3Mpa, heat up, backflow, when tower top temperature reaches 77.5 DEG C, collect cut, collection cut while again toward additional mass concentration in high-pressure rectification system be the methylal of 85%, 0.25 ~ 0.75 of this system reboiler capacity is accounted for keep this intrasystem methylal, after having entered material, stop collecting when tower top temperature reaches 77.9 DEG C, cooling, row pressure, obtaining 17500kg mass concentration is the methylal of 99.9%, liquid at the bottom of tower to be 2370kg mass concentration be 99% methyl alcohol, for the synthesis of methylal.
Embodiment 7
The methylal that certainweight mass concentration is 80% is purified, comprise the steps: by 2000kg mass concentration be first 80% methylal squeeze in high-pressure rectification system that (the reboiler capacity of distillation system is 5m3, the volume of 2000kg methylal is 2.35m3), inflated with nitrogen, keeping system pressure is 0.8Mpa, heat up, backflow, when tower top temperature reaches 117.7 DEG C, collect cut, collection cut while again toward additional mass concentration in high-pressure rectification system be the methylal of 80%, 0.25 ~ 0.75 of this system reboiler capacity is accounted for keep this intrasystem methylal, continuous seepage by this way, gained cut is through cooling, row pressure, obtaining mass concentration is the methylal of 99.9%, liquid at the bottom of gained tower to be mass concentration be 99.9% methyl alcohol, can be used for synthesizing dimethoxym ethane.
It should be noted that, above preferred embodiment is used for illustrative purposes only, but not limitation of the present invention, person skilled in the relevant technique, without departing from the spirit and scope of the present invention, done various conversion or modification, all belong to category of the present invention.
Claims (4)
1. the method for purification of a methylal, it is characterized in that comprising the steps: in the methylal of mass concentration <90%, add water and fully stir evenly, the weight that adds water is 0.2 ~ 3 times of methylal folding hundred amounts, layering is carried out after static 20 ~ 40min, add siccative in upper strata and carry out drying, and stir 5 ~ 15 minutes, its water suction weight of the siccative added is 1 ~ 12 times of methylal weight in wet base in upper strata, filter out siccative after drying and namely obtain the methylal that mass concentration is greater than 99.5%, gained lower floor is methylal, the mixture of first alcohol and water, the lower floor of rectifying at normal temperatures and pressures mixture, reclaim methylal and methyl alcohol, or in lower floor's mixture, add formaldehyde through catalyzing and synthesizing methylal, hydrous desiccant is recyclable recycling after dehydration.
2. the method for purification of a kind of methylal according to claim 1, is characterized in that: described siccative is: molecular sieve, magnesium sulfate, aluminum oxide, barium oxide, calcium oxide, calcium chloride, sodium sulfate, calcium sulfate, silica gel any one, two or more mixture.
3. the method for purification of a kind of methylal according to claim 1 and 2, it is characterized in that the methylal comprising the steps: first to add 0.25 ~ 0.75 mass concentration <95% accounting for this system reboiler capacity in high-pressure rectification system, then nitrogen is filled with, reach after 0.1 ~ 0.8Mpa until system pressure, heat up, backflow, and collect tower top temperature and reach cut within the scope of 63.5 ~ 117.7 DEG C, again toward the methylal of additional mass concentration <95% in high-pressure rectification system while collection cut, 0.25 ~ 0.75 of this system reboiler capacity is accounted for keep this intrasystem methylal, after charging completes, stop collecting when tower top temperature reaches 63.9 ~ 118.0 DEG C, the cut collected is lowered the temperature through condenser condenses, namely mass concentration >99.5% methylal is obtained after row pressure, the mixture of to be mass concentration be 99% methyl alcohol of liquid at the bottom of the tower of gained and a small amount of methylal.
4. the method for purification of a kind of methylal according to claim 3, is characterized in that: described system pressure is 0.2 ~ 0.6Mpa, and tower top temperature is 63.7 ~ 104.7 DEG C.
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| CN201510273594.8A CN104961631A (en) | 2015-05-26 | 2015-05-26 | Methylal purifying method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106397145A (en) * | 2016-09-05 | 2017-02-15 | 沈阳化工大学 | Industrial dimethoxymethane raw material dehydration process method |
| CN106397144A (en) * | 2016-09-05 | 2017-02-15 | 沈阳化工大学 | Method for removing moisture in methylal raw material |
| CN112811993A (en) * | 2020-12-29 | 2021-05-18 | 安徽省福泰精细化工有限责任公司 | Methylal purification method |
-
2015
- 2015-05-26 CN CN201510273594.8A patent/CN104961631A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106397145A (en) * | 2016-09-05 | 2017-02-15 | 沈阳化工大学 | Industrial dimethoxymethane raw material dehydration process method |
| CN106397144A (en) * | 2016-09-05 | 2017-02-15 | 沈阳化工大学 | Method for removing moisture in methylal raw material |
| CN106397144B (en) * | 2016-09-05 | 2019-04-05 | 沈阳化工大学 | A method of moisture in removal dimethoxym ethane raw material |
| CN106397145B (en) * | 2016-09-05 | 2019-04-05 | 沈阳化工大学 | A kind of industry dimethoxym ethane raw material dewatering process method |
| CN112811993A (en) * | 2020-12-29 | 2021-05-18 | 安徽省福泰精细化工有限责任公司 | Methylal purification method |
| CN112811993B (en) * | 2020-12-29 | 2023-08-25 | 安徽省福泰精细化工有限责任公司 | Methylal purification method |
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Application publication date: 20151007 |