CN105130777A - Recycling method for methanol in formaldehyde production - Google Patents

Recycling method for methanol in formaldehyde production Download PDF

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Publication number
CN105130777A
CN105130777A CN201510517615.6A CN201510517615A CN105130777A CN 105130777 A CN105130777 A CN 105130777A CN 201510517615 A CN201510517615 A CN 201510517615A CN 105130777 A CN105130777 A CN 105130777A
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China
Prior art keywords
methanol
tower
formaldehyde
rectifying
absorption
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Pending
Application number
CN201510517615.6A
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Chinese (zh)
Inventor
陶长文
周万全
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Anhui Jinhe Industrial Co Ltd
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Anhui Jinhe Industrial Co Ltd
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Publication date
Application filed by Anhui Jinhe Industrial Co Ltd filed Critical Anhui Jinhe Industrial Co Ltd
Priority to CN201510517615.6A priority Critical patent/CN105130777A/en
Publication of CN105130777A publication Critical patent/CN105130777A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/27Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation
    • C07C45/32Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen
    • C07C45/37Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups
    • C07C45/38Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by oxidation with molecular oxygen of >C—O—functional groups to >C=O groups being a primary hydroxyl group
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/78Separation; Purification; Stabilisation; Use of additives
    • C07C45/783Separation; Purification; Stabilisation; Use of additives by gas-liquid treatment, e.g. by gas-liquid absorption

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a recycling method for methanol in formaldehyde production; a formaldehyde solution after reaction in an oxidation device is subjected to formaldehyde cyclic absorption through a first-level absorption tower, a second-level absorption tower and a third-level absorption tower, a third-level absorption tower circulating liquid is subjected to partial formaldehyde cyclic absorption through a circulating pump, a part of the circulating liquid is sent into a rectifying tower, 0.25 MPa steam self-produced by the oxidation device is introduced into the rectifying tower, the circulating liquid is rectified to obtain 98% fine methanol, the 98% fine methanol is introduced into a methanol evaporator through a pipeline, residual liquid rectified out by the rectifying tower returns to the second-level absorption tower and is subjected to repeated cyclic absorption. The recycling method has the advantages that the three-tower circulating liquid is finely processed by the rectifying tower into the 98% fine methanol for reutilization, the consumption of methanol is reduced, the alcohol content in the finished product is reduced to be beneficial for production of downstream products pentaerythritol and neopentyl glycol, and the content of wastewater COD in the production process of the two products is reduced.

Description

Methanol Recovery method in Formaldehyde Production
Technical field
The present invention relates to the production field of industrial chemicals formaldehyde, the Methanol Recovery method particularly in Formaldehyde Production.
Background technology
What Formaldehyde Production adopted is silver-colored method technique, and evaporation bubbling produces two yuan of gases, and add batching vapor mixing and form ternary gas, oxidizer of making a gift to someone together with methanol steam, under silver catalyst effect, oxidative dehydrogenation occurs.When reaction transforms, have 0.5% methyl alcohol not participate in reaction and be just brought in absorption tower, cause in finished product formaldehyde and will contain methyl alcohol, methyl alcohol consumes at 445kg/t the whole year.
Summary of the invention
Object of the present invention is exactly the methyl alcohol in order to overcome containing high level in finished product formaldehyde in prior art, the Methanol Recovery method in a kind of Formaldehyde Production provided.
The technical solution used in the present invention is as follows:
A kind of Methanol Recovery method in Formaldehyde Production, after methanol steam and ternary gas enter oxidizer generation oxidative dehydrogenation, finished product formaldehyde is from dealcoholize column extraction, again through one, two, three grades of absorption tower cyclic absorption formaldehyde, it is characterized in that: a connected rectifying tower is set behind three grades of absorption towers, three grades of absorption tower circulation fluids absorb formaldehyde by recycle pump component loops, component loops liquid sends into rectifying tower, the steam of 0.25Mpa self-produced for oxidizer is incorporated into rectifying tower, the refined methanol that rectifying goes out 98% is carried out to circulation fluid, the refined methanol of 98% is incorporated into methanol evaporator by pipeline and reuses, turn back to two-level absorption tower recirculation the residual night that rectifying tower rectifying goes out to absorb.
On the basis of technique scheme, there is following further technical scheme:
The circulation fluid of first grade absorption tower is incorporated into heat exchange of methanol device, adds thermosetting methanol steam to the methyl alcohol in methyl alcohol groove.
The invention has the advantages that:
Owing to have employed technique scheme, finished product formaldehyde is from dealcoholize column extraction, three tower circulation fluids to be made a gift to someone rectifying tower precision work by recycle pump component loops, part, the recycling of processing more than 98% content refined methanol, alcohol content reduction in methanol consumption, finished product can be reduced and be conducive to derived product tetramethylolmethane, neopentyl glycol production, reduce the content of waste water cod in two process of producing product, improve product quality.
Accompanying drawing illustrates:
Fig. 1 is process flow sheet of the present invention.
Embodiment:
As shown in Figure 1, Methanol Recovery method in a kind of Formaldehyde Production provided by the invention, methanol steam and ternary gas enter oxidizer generation oxidative dehydrogenation by methanol evaporator and ternary strainer respectively simultaneously, finished product formaldehyde from dealcoholize column extraction, then passes through one, two, three absorption tower cyclic absorption formaldehyde.Absorb after formaldehyde through one-level, two-level absorption tower, in three grades of absorption towers, in circulate soln, formaldehyde content reaches 6%, methanol content reaches 5%.
A connected rectifying tower is set behind three grades of absorption towers, three grades of absorption tower circulation fluids squeeze into rectifying tower by the circulation fluid of recycle pump component loops absorption formaldehyde, wherein 1/3rd by recycle pump, the 130C of 0.25Mpa self-produced for oxidizer ° steam is incorporated into rectifying tower, to circulation fluid carry out rectifying obtain 98% refined methanol (distillation is common process, distillation parameter is omitted), the refined methanol of 98% is incorporated into methanol evaporator by pipeline and reuses.The raffinate that rectifying tower rectifying goes out content 1% formalin gets back to two towers, three tower cyclic absorption, ensures that catalyst uses methanol content less than 0.2% in the initial stage to finished product formaldehyde during replacing catalyst, reduces methanol consumption.
The temperature of the circulation fluid of first grade absorption tower is 90C °, in circulation fluid containing 14% formaldehyde, 0.5% methyl alcoholthe aqueous solution, it can be used as thermal source to be incorporated into heat exchange of methanol device, is heated to more than 60C ° forms methanol steam to the methyl alcohol in methyl alcohol groove, enters oxidizer participate in reaction by methanol evaporator.

Claims (2)

1. the Methanol Recovery method in Formaldehyde Production, comprise after methanol steam and ternary gas enter oxidizer generation oxidative dehydrogenation, finished product formaldehyde is from dealcoholize column extraction, again through one, two, three grades of absorption tower cyclic absorption formaldehyde, it is characterized in that: a connected rectifying tower is set behind three grades of absorption towers, three grades of absorption tower circulation fluids absorb formaldehyde by recycle pump component loops, component loops liquid sends into rectifying tower, the steam of 0.25Mpa self-produced for oxidizer is incorporated into rectifying tower, the refined methanol that rectifying goes out 98% is carried out to circulation fluid, the refined methanol of 98% is incorporated into methanol evaporator by pipeline, turn back to two-level absorption tower recirculation the residual night that rectifying tower rectifying goes out to absorb.
2. the Methanol Recovery method in Formaldehyde Production according to claim 1, is characterized in that:
The circulation fluid of first grade absorption tower is incorporated into heat exchange of methanol device, adds thermosetting methanol steam to the methyl alcohol of the inflow in methyl alcohol groove.
CN201510517615.6A 2015-08-22 2015-08-22 Recycling method for methanol in formaldehyde production Pending CN105130777A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510517615.6A CN105130777A (en) 2015-08-22 2015-08-22 Recycling method for methanol in formaldehyde production

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510517615.6A CN105130777A (en) 2015-08-22 2015-08-22 Recycling method for methanol in formaldehyde production

Publications (1)

Publication Number Publication Date
CN105130777A true CN105130777A (en) 2015-12-09

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510517615.6A Pending CN105130777A (en) 2015-08-22 2015-08-22 Recycling method for methanol in formaldehyde production

Country Status (1)

Country Link
CN (1) CN105130777A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106349043A (en) * 2016-08-30 2017-01-25 安徽金禾实业股份有限公司 Attenuant acetaldehyde rectification residual liquor recycling method
CN109574820A (en) * 2018-12-10 2019-04-05 安徽金禾实业股份有限公司 A kind of production method of formaldehyde
CN110330418A (en) * 2019-06-20 2019-10-15 湖北楚星化工股份有限公司 A method of recycling the formaldehyde gas to volatilize in atmospheric unit in Production of pentaerythritol
CN110721554A (en) * 2019-11-19 2020-01-24 安徽金禾实业股份有限公司 Comprehensive utilization method for pentaerythritol production wastewater and formaldehyde acetaldehyde
CN112920029A (en) * 2021-02-03 2021-06-08 安徽金禾实业股份有限公司 Device and method for extracting and refining methanol from formaldehyde

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106349043A (en) * 2016-08-30 2017-01-25 安徽金禾实业股份有限公司 Attenuant acetaldehyde rectification residual liquor recycling method
CN106349043B (en) * 2016-08-30 2018-11-06 安徽金禾实业股份有限公司 A kind of dilute acetaldehyde distillation residual liquid recycling application method
CN109574820A (en) * 2018-12-10 2019-04-05 安徽金禾实业股份有限公司 A kind of production method of formaldehyde
CN109574820B (en) * 2018-12-10 2021-12-21 安徽金禾实业股份有限公司 Production method of formaldehyde
CN110330418A (en) * 2019-06-20 2019-10-15 湖北楚星化工股份有限公司 A method of recycling the formaldehyde gas to volatilize in atmospheric unit in Production of pentaerythritol
CN110330418B (en) * 2019-06-20 2022-03-15 湖北楚星化工股份有限公司 Method for recovering formaldehyde gas volatilized in normal pressure device in pentaerythritol production
CN110721554A (en) * 2019-11-19 2020-01-24 安徽金禾实业股份有限公司 Comprehensive utilization method for pentaerythritol production wastewater and formaldehyde acetaldehyde
CN112920029A (en) * 2021-02-03 2021-06-08 安徽金禾实业股份有限公司 Device and method for extracting and refining methanol from formaldehyde

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Application publication date: 20151209

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