CN109503409A - Sucralose is esterified reaction acid DMF processing method and processing device - Google Patents
Sucralose is esterified reaction acid DMF processing method and processing device Download PDFInfo
- Publication number
- CN109503409A CN109503409A CN201811504146.4A CN201811504146A CN109503409A CN 109503409 A CN109503409 A CN 109503409A CN 201811504146 A CN201811504146 A CN 201811504146A CN 109503409 A CN109503409 A CN 109503409A
- Authority
- CN
- China
- Prior art keywords
- rectifying column
- dmf
- methanol
- reboiler
- tower
- Prior art date
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/22—Separation; Purification; Stabilisation; Use of additives
- C07C231/24—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of Sucraloses to be esterified reaction acid DMF processing method and processing device, it is characterized by: a. DMF containing acetic acid, sulfuric acid, methanol enter rectifying column one (4), 125-135 DEG C of temperature in tower, gas partial reflux after condenser (5), remaining enters methyl acetate pan tank (10), kettle material is after reboiler one (7) heating, part is back to rectifying column, remaining through valve tower (11), pre-heater (19), reboiler two (12) enters back into rectifying column two (18) after recycling methanol into raffinate slot (9)；B. interior 100-110 DEG C of temperature of rectifying column two (18) are controlled, for gas after condenser (13) condense, part returns to rectifying column two (18), remaining DMF is into DMF pan tank (15), for kettle material after reboiler three (17), gas returns to tower reactor, remaining enters raffinate slot (16).The invention has the advantages that simple process, easily operated；Reduce sewage treatment difficulty and cost, sewage zero-discharge；DMF is recycled to greatest extent；Obtain methyl acetate.
Description
Technical field
The invention belongs to chemical technology fields, are related to Sucralose production field, and in particular to a kind of Sucralose esterification is anti-
Answer acid DMF processing method and processing device.
Background technique
In Sucralose production, as first step esterification using be added DMF, catalyst organotin acetic acid esters it is de-
Water reaction is extracted after the reaction was completed plus after aceticanhydride reaction with extractant hexamethylene, after being concentrated in the DMF phase separated
In DMF contain a large amount of acetic acid, prior art by add 32% sodium hydroxide solution carry out neutralize produce sodium acetate crude product after
It is purified, entire neutralisation treatment process cost is high, and pollution is big, and ammonia nitrogen and COD are difficult in mother liquor, are directly discharged into wastewater trough
The processing of decontamination water station, brings great difficulty to sewage treatment.
Summary of the invention
The purpose of the present invention is to solve acidity DMF processing pollution after the esterification reaction of existing Sucralose is big, at high cost
The problem of, a kind of Sucralose esterification reaction acid DMF processing method and processing device is provided.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of Sucralose esterification reaction acid DMF processing unit, it is characterised in that including following equipment: one bottom of rectifying column goes out
Mouth is connected by reboiler one, raffinate slot one, valve tower, pre-heater, reboiler two with two centre entrance of rectifying column, rectifying column
Two outlet at bottom are connected to raffinate slot two by reboiler three；
One upper, middle and lower entrance of rectifying column is connected with acetic acid DMF slot, sulfuric acid tank, methanol slot respectively, and one top exit of rectifying column is logical
Cross at the top of condenser one, counter flow controller one and rectifying column one and be connected, another outlet of counter flow controller one and methyl acetate at
Product slot is connected；Another outlet in one bottom of rectifying column is connected to one top of rectifying column by pipeline, and boiling device one is connected with steam generator,
One top exit of reboiler is connected to one bottom of rectifying column by pipeline；
Two top exit of rectifying column at the top of condenser two, counter flow controller two and rectifying column two by being connected, counter flow controller two
Another outlet be connected with DMF pan tank；Another outlet in two bottom of rectifying column is connected to two top of rectifying column, reboiler by pipeline
Three top exits are connected to two bottom of rectifying column by pipeline, and another outlet of reboiler three is connected in the middle part of rectifying column one by pipeline
Mouthful.
A kind of Sucralose esterification reaction acid DMF processing method, it is characterised in that the following steps are included:
A. DMF containing acetic acid, sulfuric acid, the methanol after esterification concentration are sent into rectifying column one by pipeline respectively, make DMF containing acetic acid
With methanol counter current contacting, controlling acetic acid DMF, sulfuric acid, methanol volume ratio is 2:0.3:1, and controlling temperature in rectifying column one is 125-
135 DEG C, rectifying column 123-128 DEG C of gas of one tower top temperature (methyl acetate) is after condenser condenses, control section methyl acetate
In reflux (reflux ratio is 1~6) to rectifying column one, remaining methyl acetate enters methyl acetate pan tank, one tower reactor object of rectifying column
(aqueous DMF, methanol, sulfuric acid) is expected after reboiler one is heated to 60-70 DEG C, methanol, sulfuric acid are back to rectifying column, aqueous DMF,
Methanol enters raffinate slot recycling methanol, subsequent aqueous DMF pumped after valve tower (- 0.086~-0.092MPa) removes moisture to
Pre-heater carries out being preheated to 105-108 DEG C, enters back into reboiler two and is heated to 110 ± 5 DEG C；
B. the DMF(after pre-heater preheats contains methanol) the progress rectifying of rectifying column two is entered back into, control temperature in rectifying column two
100-110 DEG C, 90-95 DEG C of tower top temperature, overhead gas (DMF, methanol) after condenser is condensed to 3~8 DEG C, control methanol,
The return of DMF liquid (reflux ratio are as follows: 1~6) in rectifying column two, remaining DMF(liquid) enter DMF pan tank, kettle material (first
Alcohol) after reboiler three is heated to 60-70 DEG C, gas methanol returns to tower reactor, remaining methanol enters raffinate slot.
Further, the reflux ratio of rectifying column two can also be 5.1-6 in rectifying column one and step b in the step a.
By the DMF containing acetic acid after esterification concentration, rectifying column is added by different positions respectively in methanol, sulfuric acid (catalyst)
It is interior, make DMF containing acetic acid and methanol counter current contacting, stripping section is mainly the separation of methanol Yu aqueous DMF, the first risen from stripping section
Alcohol steam and the acetic acid of rectifying section decline carry out counter current contacting in conversion zone and generate methyl acetate and water, and wherein acetic acid is in decline
It had not only been used as reactant in the process but also has been used as extractant, the methanol extracted and acetic acid generate a small amount of methyl acetate again, with laggard
Row separation extraction methyl acetate, last aqueous DMF, methanol, sulfuric acid are flowed out from one tower reactor of rectifying column, and sulfuric acid and water are from tower reactor stream
Out, DMF, methanol are using two rectifying of rectifying column, two tower top of rectifying column separation extraction DMF, two tower reactor of rectifying column extraction methanol.
The invention has the advantages that methanol is entered reactive distillation together with the mixed liquor of DMF containing acetic acid and catalyst and produces height by 1.
The DMF of purity makes acetic acid be converted into methyl acetate simultaneously, simple process, easily operated；2. reducing sewage treatment and solid waste
Processing difficulty has accomplished that sewage zero-discharge is generated without solid waste；3. recycling DMF purity reaches 99.5% and returns to greatest extent
Workshop section is gone back to use again；4. obtained methyl acetate improves economic benefit and substantially reduces production cost.
Detailed description of the invention
Fig. 1 is that Sucralose is esterified reaction acid DMF processing technological flow schematic diagram.
Specific embodiment
In conjunction with Fig. 1, a kind of Sucralose is esterified reaction acid DMF processing method and processing device, and specific implementation step is as follows:
A kind of Sucralose esterification reaction acid DMF processing unit, including following equipment: rectifying column one (4) outlet at bottom passes through
In reboiler one (7), raffinate slot one (9), valve tower (11), pre-heater (19), reboiler two (12) and rectifying column two (18)
Portion's entrance is connected, and rectifying column two (18) outlet at bottom is connected to raffinate slot two (16) by reboiler three (17)；
Rectifying column one (4) upper, middle and lower entrance is connected with acetic acid DMF slot (1), sulfuric acid tank (2), methanol slot (3) respectively, rectifying column
One (4) top exit at the top of condenser one (5), counter flow controller one (6) and rectifying column one (4) by being connected, counter flow controller
Another outlet of one (6) is connected with methyl acetate pan tank (10)；Another outlet in rectifying column one (4) bottom is connected to essence by pipeline
It evaporates at the top of tower one (4), boiling device one (7) is connected with steam generator (8), and reboiler one (7) top exit is connected to essence by pipeline
Evaporate tower one (4) bottom；
Rectifying column two (18) top exit passes through condenser two (13), counter flow controller two (14) and phase at the top of rectifying column two (18)
Even, another outlet of counter flow controller two (14) is connected with DMF pan tank (15)；Another outlet in rectifying column two (18) bottom passes through
Pipeline is connected at the top of rectifying column two (18), and reboiler three (17) top exit is connected to rectifying column two (18) bottom by pipeline, then
Another outlet of boiling device three (17) is connected to rectifying column one (4) centre entrance by pipeline.
Embodiment 1
A, DMF containing acetic acid 2000L, sulfuric acid 330L, 1000 L of methanol after esterification concentration are passed through pipeline respectively and is sent into rectifying column
In one (4), make DMF containing acetic acid and methanol counter current contacting, control rectifying column one (4) head temperature is 126 ± 2 DEG C, rectifying column one
(4) for overhead gas (methyl acetate) after condenser (5) condense 3~8 DEG C, control section methyl acetate flows back (reflux ratio 2)
In to rectifying column one (4), remaining methyl acetate enters methyl acetate pan tank (10)；
B, rectifying column one (4) kettle material (aqueous DMF, methanol, sulfuric acid) is after reboiler one (7) heats 65 DEG C, methanol, sulfuric acid
It is back to rectifying column, aqueous DMF, methanol enter raffinate slot (9) recycling, first recycles a large amount of methanol and go to methanol slot (3), will be aqueous
DMF is pumped to valve tower (11), and the valve tower is that the vacuum of negative pressure -0.086MPa makes operative liquid water evaporation, will then be divided
The DMF liquid that water tower (11) comes out is pumped to pre-heater (19) and carries out 105-108 DEG C of preheating,；
C. the DMF(after pre-heater (19) preheating contains methanol) it pumps to reboiler (12) and is heated to 110 ± 5 DEG C, then will
The DMF that heater comes out is pumped to rectifying column two (18), and tower top temperature maintains 92 ± 1 DEG C, and bottom temperature maintains 106 ± 2
DEG C, so that liquid water is evaporated and is separated from DMF recovered liquid, overhead gas (DMF, methanol) condenses 3~8 DEG C through condenser (13)
Afterwards, methanol is controlled, DMF liquid returns in rectifying column two (18) (reflux ratio 5), remaining DMF(liquid) enter DMF pan tank
(15)；
D, after reboiler three (17) heats 65 DEG C, gas methanol returns in one tower reactor of rectifying column kettle material (methanol), remaining
Methanol enters raffinate slot (16).
The DMF containing acetic acid that this technique generates process is reacted by methanol esterification removes acetic acid, and maximum recycling DMF is returned
Production line uses, and reacts obtained ethyl acetate finished product and obtains effective economic benefit.Original traditional handicraft is by after DMF rectifying points
It is neutralized from Dichlorodiphenyl Acetate after depickling and produces sodium acetate, at high cost, pollution is big, and mother liquor is difficult to be directly discharged at waste water
Reason station.Accomplish zero-emission in entire production process now, first carries out directly rectifying qualification DMF after deacidification reaction.
Claims (5)
1. a kind of Sucralose is esterified reaction acid DMF processing unit, it is characterised in that including following equipment: rectifying column one (4)
Outlet at bottom passes through reboiler one (7), raffinate slot one (9), valve tower (11), pre-heater (19), reboiler two (12) and essence
It evaporates tower two (18) centre entrance to be connected, rectifying column two (18) outlet at bottom is connected to raffinate slot two (16) by reboiler three (17)；
Rectifying column one (4) upper, middle and lower entrance is connected with acetic acid DMF slot (1), sulfuric acid tank (2), methanol slot (3) respectively, rectifying column
One (4) top exit at the top of condenser one (5), counter flow controller one (6) and rectifying column one (4) by being connected, counter flow controller
Another outlet of one (6) is connected with methyl acetate pan tank (10)；Another outlet in rectifying column one (4) bottom is connected to essence by pipeline
It evaporates at the top of tower one (4), reboiler one (7) is connected with steam generator (8), and reboiler one (7) top exit is connected to by pipeline
Rectifying column one (4) bottom；
Rectifying column two (18) top exit passes through condenser two (13), counter flow controller two (14) and phase at the top of rectifying column two (18)
Even, another outlet of counter flow controller two (14) is connected with DMF pan tank (15)；Another outlet in rectifying column two (18) bottom passes through
Pipeline is connected at the top of rectifying column two (18), and reboiler three (17) top exit is connected to rectifying column two (18) bottom by pipeline, then
Another outlet of boiling device three (17) is connected to rectifying column one (4) centre entrance by pipeline.
2. a kind of Sucralose is esterified reaction acid DMF processing method, it is characterised in that the following steps are included:
A. DMF containing acetic acid, sulfuric acid, the methanol after esterification concentration are sent into rectifying column one (4) by pipeline respectively, are made containing acetic acid
DMF and methanol counter current contacting, control acetic acid DMF, sulfuric acid, methanol volume ratio are 2:0.3:1, control rectifying column one (4) interior temperature
It is 125-135 DEG C, 123-128 DEG C of gas of rectifying column one (4) tower top temperature is after condenser (5) condense, control section tumer
Ester is back in rectifying column one (4), remaining methyl acetate enters methyl acetate pan tank (10), rectifying column one (4) kettle material
After reboiler one (7) is heated to 60-70 DEG C, methanol, sulfuric acid are back to rectifying column, and aqueous DMF, methanol enter raffinate slot (9)
A large amount of methanol are recycled, subsequent aqueous DMF is pumped to pre-heater (19) after valve tower (11) remove moisture and is preheated to 105-
It 108 DEG C, enters back into reboiler two (12) and is heated to 110 ± 5 DEG C；
B. the DMF after pre-heater (19) preheating and methanol enter back into rectifying column two (18) and carry out rectifying, control rectifying column two
(18) 100-110 DEG C of interior temperature, 90-95 DEG C of tower top temperature, overhead gas controls first after condenser (13) are condensed to 3~8 DEG C
Alcohol, DMF liquid return in rectifying column two (18), remaining DMF enters DMF pan tank (15), and kettle material is through reboiler three (17)
After being heated to 60-70 DEG C, gas methanol returns to tower reactor, remaining methanol enters raffinate slot (16).
3. a kind of Sucralose is esterified reaction acid DMF processing method according to claim 2, it is characterised in that: in step a
The reflux ratio of rectifying column two (18) is 1~6 in rectifying column one (4) and step b.
4. a kind of Sucralose is esterified reaction acid DMF processing method according to claim 2, it is characterised in that: in step a
The reflux ratio of rectifying column two (18) can also be 5.1-6 in rectifying column one (4) and step b.
5. a kind of Sucralose is esterified reaction acid DMF processing method according to claim 2, it is characterised in that: in step a
The pressure of valve tower (11) is -0.086~-0.092MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811504146.4A CN109503409A (en) | 2018-12-10 | 2018-12-10 | Sucralose is esterified reaction acid DMF processing method and processing device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811504146.4A CN109503409A (en) | 2018-12-10 | 2018-12-10 | Sucralose is esterified reaction acid DMF processing method and processing device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109503409A true CN109503409A (en) | 2019-03-22 |
Family
ID=65752062
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811504146.4A Pending CN109503409A (en) | 2018-12-10 | 2018-12-10 | Sucralose is esterified reaction acid DMF processing method and processing device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109503409A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592469A (en) * | 2020-05-22 | 2020-08-28 | 安徽金禾实业股份有限公司 | Method for recovering DMAC (dimethylacetamide) residual liquid in sucralose production |
| CN111606822A (en) * | 2020-05-25 | 2020-09-01 | 安徽金禾实业股份有限公司 | Method for recovering acidic DMF (dimethyl formamide) in sucralose production |
| CN113636951A (en) * | 2021-09-22 | 2021-11-12 | 安徽金禾实业股份有限公司 | Method for treating waste DMF in sucralose production |
| CN113666838A (en) * | 2021-09-22 | 2021-11-19 | 安徽金禾实业股份有限公司 | Method for recovering low-concentration DMF (dimethyl formamide) through double-tower coupling in sucralose production |
| CN115677527A (en) * | 2022-11-17 | 2023-02-03 | 安徽金禾实业股份有限公司 | Method for purifying acidic DMF in sucralose production |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1097254A (en) * | 1976-08-18 | 1981-03-10 | Norman A. Portnoy | Recovery of chemical components of cellulosic regenerating solution |
| CN1919821A (en) * | 2006-09-13 | 2007-02-28 | 西南化工研究设计院 | Method of recovery acetic acid from acetic acid containing waste water |
| CN102070478A (en) * | 2011-01-14 | 2011-05-25 | 常州大学 | Method for recycling dimethylformamide in water through pervaporation and rectification coupling technology |
| CN106831471A (en) * | 2017-01-20 | 2017-06-13 | 福州大学 | A kind of method for removing a small amount of acid or glacial acetic acid and refining DMF |
-
2018
- 2018-12-10 CN CN201811504146.4A patent/CN109503409A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1097254A (en) * | 1976-08-18 | 1981-03-10 | Norman A. Portnoy | Recovery of chemical components of cellulosic regenerating solution |
| CN1919821A (en) * | 2006-09-13 | 2007-02-28 | 西南化工研究设计院 | Method of recovery acetic acid from acetic acid containing waste water |
| CN102070478A (en) * | 2011-01-14 | 2011-05-25 | 常州大学 | Method for recycling dimethylformamide in water through pervaporation and rectification coupling technology |
| CN106831471A (en) * | 2017-01-20 | 2017-06-13 | 福州大学 | A kind of method for removing a small amount of acid or glacial acetic acid and refining DMF |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111592469A (en) * | 2020-05-22 | 2020-08-28 | 安徽金禾实业股份有限公司 | Method for recovering DMAC (dimethylacetamide) residual liquid in sucralose production |
| CN111606822A (en) * | 2020-05-25 | 2020-09-01 | 安徽金禾实业股份有限公司 | Method for recovering acidic DMF (dimethyl formamide) in sucralose production |
| CN113636951A (en) * | 2021-09-22 | 2021-11-12 | 安徽金禾实业股份有限公司 | Method for treating waste DMF in sucralose production |
| CN113666838A (en) * | 2021-09-22 | 2021-11-19 | 安徽金禾实业股份有限公司 | Method for recovering low-concentration DMF (dimethyl formamide) through double-tower coupling in sucralose production |
| CN115677527A (en) * | 2022-11-17 | 2023-02-03 | 安徽金禾实业股份有限公司 | Method for purifying acidic DMF in sucralose production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109503409A (en) | Sucralose is esterified reaction acid DMF processing method and processing device | |
| CN101735045B (en) | Method for producing ethyl acetate by using entrainer | |
| CN103566613A (en) | Rectification device and process for low-concentration organic solvent aqueous liquor recycling heat pump | |
| CN112608232B (en) | System and method for recycling reaction heat in process of synthesizing acetic acid by methanol low-pressure carbonyl | |
| CN102295564A (en) | Continuous production process for DOP (Dioctyl Phthalate) and used equipment | |
| CN108059597A (en) | A kind of reactive distillation integrates the method and its device of production ethyl acetate with infiltration evaporation | |
| CN101704839A (en) | High purity triisobutyl phosphate preparation technology | |
| CN109503410A (en) | The method of solvent DMF recycling in a kind of production of Sucralose | |
| CN107827779A (en) | Batch reactive distillation production cyanoacetate compound, malonate compound device and its production technology | |
| CN106478415B (en) | A kind of ethyl acetate energy-saving processing technique | |
| CN103524478B (en) | Device and method for shortening ketalation time in ibuprofen synthesis process | |
| CN110526814A (en) | The method that serialization prepares butyric acid | |
| CN103848864A (en) | Preparation process of high-purity triisobutyl phosphate | |
| CN102675098A (en) | New process for continuous production of butyl acrylate | |
| CN111592469A (en) | Method for recovering DMAC (dimethylacetamide) residual liquid in sucralose production | |
| CN105669445B (en) | The production technology of ethyl acetate | |
| MX2012010806A (en) | Method for producing a carboxylic acid ester. | |
| CN101596371B (en) | Device for purifying formic acid solution with interval azeotropic distillation and method thereof | |
| CN107501093A (en) | A kind of device and method of partition wall reactive distillation column production ethylene acetate | |
| CN103467299B (en) | The preparation method and device of methyl nitrite in a kind of synthesis gas preparing ethylene glycol technique | |
| CN107011159B (en) | The processing method and processing device of residue in a kind of acetic acid refining and recovery system | |
| CN104829452B (en) | Energy-saving production system of ethyl acetate and corresponding energy-saving production technology | |
| CN207537374U (en) | Batch reactive distillation production cyanoacetate compound, malonate compound device | |
| CN101747177A (en) | Device and method for preparing butane diacid by continuously hydrolyzing dialkyl succinate ester | |
| CN107141199A (en) | Methanol mother liquor is without refluxed cryogenic rectificating method and equipment |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190322 |
|
| RJ01 | Rejection of invention patent application after publication |