CN112624910A - Production method of diethylene glycol dimethyl ether - Google Patents
Production method of diethylene glycol dimethyl ether Download PDFInfo
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- CN112624910A CN112624910A CN202110039909.8A CN202110039909A CN112624910A CN 112624910 A CN112624910 A CN 112624910A CN 202110039909 A CN202110039909 A CN 202110039909A CN 112624910 A CN112624910 A CN 112624910A
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- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 96
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- 239000000047 product Substances 0.000 claims abstract description 32
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 230000018044 dehydration Effects 0.000 claims abstract description 27
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 27
- 238000011084 recovery Methods 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 25
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 claims abstract description 22
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 20
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 14
- 229940050176 methyl chloride Drugs 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000011780 sodium chloride Substances 0.000 claims abstract description 10
- 239000002910 solid waste Substances 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 11
- 239000002351 wastewater Substances 0.000 claims description 11
- 230000008859 change Effects 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 239000012043 crude product Substances 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000002699 waste material Substances 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims 1
- 238000009833 condensation Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000009835 boiling Methods 0.000 abstract description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 4
- YCRYSVKEWAWTGI-UHFFFAOYSA-N p,p'-Methoxychlor olefin Chemical compound C1=CC(OC)=CC=C1C(=C(Cl)Cl)C1=CC=C(OC)C=C1 YCRYSVKEWAWTGI-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- ZTOPSBJLVPWTGF-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol;sodium Chemical compound [Na].COCCOCCO ZTOPSBJLVPWTGF-UHFFFAOYSA-N 0.000 description 2
- 238000006266 etherification reaction Methods 0.000 description 2
- 238000007327 hydrogenolysis reaction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 229920001744 Polyaldehyde Polymers 0.000 description 1
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- JLGLQAWTXXGVEM-UHFFFAOYSA-N triethylene glycol monomethyl ether Chemical compound COCCOCCOCCO JLGLQAWTXXGVEM-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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Classifications
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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
- C07C41/01—Preparation of ethers
- C07C41/18—Preparation of ethers by reactions not forming ether-oxygen bonds
- C07C41/26—Preparation of ethers by reactions not forming ether-oxygen bonds by introduction of hydroxy or O-metal groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/02—Settling tanks with single outlets for the separated liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/16—Preparation of ethers by reaction of esters of mineral or organic acids with hydroxy or O-metal groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/18—Preparation of ethers by reactions not forming ether-oxygen bonds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a production method of diethylene glycol dimethyl ether, which comprises four parallel reaction kettles, a settling tank, a pre-separation tower, a dehydration tower, a finished product tower and a solvent recovery tower, wherein the upper end surfaces of the four reaction kettles are respectively provided with a diethylene glycol methyl ether input passage, a sodium hydroxide input passage and an excess diethylene glycol methyl ether reuse passage, the lower end surfaces of the four reaction kettles are respectively provided with a methyl chloride input passage and a reaction liquid output passage, all raw materials are fully reacted in the reaction kettles, then enter the settling tank for standing and settling to separate out solid waste sodium chloride, and then are rectified and separated step by using the pre-separation tower, the dehydration tower, the finished product tower and the solvent recovery tower according to different boiling points of all components contained in supernatant liquid, so that finished product diethylene glycol dimethyl ether is finally obtained, and the added excess raw material diethylene glycol methyl ether is reused in the reaction kettles; the invention has the advantages of reasonable process route design and high production efficiency, and can quickly and accurately judge whether the reaction in the reaction kettle is finished or not through the spotlight and the photodiode array.
Description
Technical Field
The invention belongs to the technical field of chemical solvent product production, and particularly relates to a production method of diethylene glycol dimethyl ether.
Background
Diethylene glycol dimethyl ether (DMDE) is colorless neutral liquid with ether smell, has a boiling point of 162 ℃, a relative density of 0.9467 and a refractive index of 1.4097, is stable in chemical property, is not easy to react chemically, can dissolve various resins and cellulose, can be mixed and dissolved with water and a plurality of organic solvents such as alcohol, ether, ketone, ester, hydrocarbon, chlorohydrocarbon and the like in any proportion, and the dissolving capacity of the diethylene glycol dimethyl ether can be adjusted by properly diluting water or certain solvents. DMDE has many uses in organic synthesis, as an alkali metal hydroxide solvent in metal organic compound synthesis, alkylation, polycondensation, and reduction reactions, and has a wide range of applications.
At present, DMDE is synthesized by a plurality of process routes, including hydrogenolysis of triethylene glycol monomethyl ether, hydrogenolysis of diethylene glycol ether polyaldehyde, dehydration of ethylene glycol monomethyl ether, etherification reaction of diethylene glycol or the monomethyl ether thereof, reaction of dimethyl ether and ethylene oxide and the like, wherein the etherification reaction of diethylene glycol or the monomethyl ether thereof is most ideal, the process is simple, and the operation is simple, convenient and safe; but has the problems that the process route is not designed reasonably and the production efficiency is influenced; in order to solve the above problems, it is necessary to develop a method for producing diethylene glycol dimethyl ether.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the method for producing the diethylene glycol dimethyl ether, which has reasonable process route design and high production efficiency.
The purpose of the invention is realized as follows: a production method of diethylene glycol dimethyl ether comprises four reaction kettles, a settling tank, a pre-separation tower, a dehydration tower, a finished product tower and a solvent recovery tower which are arranged in parallel, wherein the upper end surfaces of the four reaction kettles are respectively provided with a common diethylene glycol methyl ether input passage, a sodium hydroxide input passage and an excess diethylene glycol methyl ether reuse passage, the lower end surfaces of the four reaction kettles are respectively provided with a common methyl chloride input passage and a reaction liquid output passage, a certain amount of diethylene glycol methyl ether is firstly conveyed into the four reaction kettles by a pump through the diethylene glycol methyl ether input passage, then a certain amount of sodium hydroxide is put into the four reaction kettles in batches through the sodium hydroxide input passage, simultaneously stirrers in the four reaction kettles are started, after the sodium hydroxide is completely dissolved and reacts and the reaction temperature in the four reaction kettles is not increased any more, a vacuum pump arranged behind the four reaction kettles is started, the metered methyl chloride is slowly introduced into the bottoms of the four reaction kettles through the methyl chloride input passage, starting reaction, discharging a reaction crude product into a settling tank through a reaction liquid output passage until the reaction is finished, standing for a certain time, conveying upper clear liquid in the settling tank to a pre-separation tower by a pump for rectification, discharging solid waste sodium chloride from the bottom of the settling tank, conveying materials at the top of the pre-separation tower to a dehydration tower by a pump after being condensed, conveying materials at the bottom of the pre-separation tower to a solvent recovery tower by a pump for continuous rectification, collecting waste water at the top of the solvent recovery tower, recycling excessive diethylene glycol monomethyl ether in materials at the bottom of the solvent recovery tower to four reaction kettles, continuously rectifying condensate by the dehydration tower, collecting waste water at the top of the dehydration tower, conveying materials at the bottom of the dehydration tower to a finished product tower by a pump for rectification, collecting finished product diethylene glycol dimethyl ether at the top of the finished product tower, and leaving a small amount of residual liquid at the bottom of the finished product tower, wherein the waste water and the residual liquid are conveyed to.
Preferably, the chemical reaction in the reaction kettle is as follows:
CH3OCH2CH2OCH2CH2OH+NaOH=CH3OCH2CH2OCH2CH2ONa+H2O；
CH3OCH2CH2OCH2CH2ONa+CH3Cl=CH3OCH2CH2OCH2CH2OCH3+NaCl↓；
preferably, the side wall of the reaction kettle is provided with a transparent window, the turbidity change of the reaction liquid in the reaction kettle is regularly observed through the transparent window, and the reaction in the reaction kettle is judged to be finished when the turbidity of the reaction liquid is basically not changed any more.
Further preferably, reation kettle's lateral wall distance position department of transparent window certain interval is equipped with the altitude mixture match the spotlight that transparent window set up, the lamp holder orientation of spotlight transparent window sets up, be equipped with on the transparent window and aim at the photodiode array that the spotlight lamp holder set up, the spotlight with light path between the photodiode array with the setting of other parts mutually noninterfere that sets up in the reation kettle, work as the photocurrent that the photodiode array detected is judged to be the reation kettle in the end when no longer changing basically.
Preferably, the reaction kettle is an intermittent reaction kettle, and the working state of the reaction kettle is T = 25-50 ℃ and P = -0.1-0.6 MPa.
Preferably, the settling tank is an intermittent settling tank, and the working state of the settling tank is T = 25-50 ℃ and P = 0-0.6 MPa.
Preferably, the pre-separation tower, the dehydration tower, the finished product tower and the dissolution recovery tower adopt rectification towers, the rectification conditions of the pre-separation tower are T = 75-110 ℃ and P = -0.1-0.2 MPa, the rectification conditions of the dehydration tower are T = 80-100 ℃ and P = -0.1-0.2 MPa, the rectification conditions of the finished product tower are T = 85-100 ℃ and P = -0.1-0.2 MPa, and the rectification conditions of the solvent recovery tower are T = 100-130 ℃ and P = -0.1-0.2 MPa.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
(1) the method adopts four reaction kettles, a settling tank, a pre-separation tower, a dehydration tower, a finished product tower and a solvent recovery tower which are arranged in parallel, after all raw materials are fully reacted in the reaction kettles, the raw materials enter the settling tank to be kept still for settling and separating out solid waste sodium chloride, then the raw materials are rectified and separated step by the pre-separation tower, the dehydration tower, the finished product tower and the solvent recovery tower according to different boiling points of all components contained in supernatant liquid, finally the finished product diethylene glycol dimethyl ether is obtained, the added excessive raw material diethylene glycol dimethyl ether is reused in the reaction kettles, the process route is reasonable in design, the product is obtained from the input of the reaction raw materials, and the production efficiency is effectively ensured;
(2) according to the invention, the setting of the settling tank for single settling volume to match with four reaction kettles is adopted, so that on one hand, a single reaction kettle with small volume can effectively ensure high reaction speed and complete reaction, and on the other hand, a single settling tank can reduce the floor area of equipment, improve the utilization efficiency of the equipment and accelerate the production progress;
(3) the invention adopts the spotlight and the photodiode array, the spotlight can help the transparent window to check the reaction condition in the reaction kettle more simply and intuitively, simultaneously, the light emitted by the spotlight is converted into photocurrent by the photodiode array, and whether the reaction in the reaction kettle is finished can be judged more accurately and quickly through the change of the photocurrent;
in summary, the invention has the advantages of reasonable process route design and high production efficiency.
Drawings
FIG. 1 is a schematic diagram of the composition structure of the present invention.
FIG. 2 is a schematic top view showing the relative positional relationship among the reaction vessel, the spotlight, the photodiode array and the stirrer (stirring shaft).
FIG. 3 is a schematic front view of the reaction kettle, the spotlight, the photodiode array and the stirrer (stirring shaft + stirring blade) according to the present invention.
In the figure: 1. the device comprises a reaction kettle 2, a vacuum pump 3, a settling tank 4, a pre-separation tower 5, a dehydration tower 6, a finished product tower 7, a solvent recovery tower 8, a spotlight 9, a photodiode array 10, a transparent window 11, a stirrer a, a diethylene glycol monomethyl ether input passage b, a sodium hydroxide input passage c, a methyl chloride input passage d, an excess diethylene glycol monomethyl ether reuse passage e, a reaction liquid output passage f, a dehydration tower top wastewater output g, a finished product tower top finished product diethylene glycol dimethyl ether output h, a finished product tower kettle residual liquid output i, a solvent recovery tower top wastewater output j, a solvent recovery tower excess diethylene glycol monomethyl ether reuse k, a solid waste sodium chloride output m, and a light path between the spotlight and the photodiode array.
Detailed Description
The technical scheme of the invention is further specifically described below with reference to the accompanying drawings.
As shown in the figure, the invention provides a production method of diethylene glycol dimethyl ether, which comprises four reaction kettles 1, a settling tank 3, a pre-separation tower 4, a dehydration tower 5, a finished product tower 6 and a solvent recovery tower 7 which are arranged in parallel, wherein the upper end surfaces of the four reaction kettles 1 are respectively provided with a common diethylene glycol methyl ether input passage a, a sodium hydroxide input passage b and an excessive diethylene glycol methyl ether reuse passage d, and the lower end surfaces of the four reaction kettles 1 are respectively provided with a common methyl chloride input passage c and a reaction liquid output passage e.
Firstly, a certain amount of diethylene glycol methyl ether is conveyed into four reaction kettles 1 by a pump through a diethylene glycol methyl ether input passage a, then a certain amount of sodium hydroxide is put into the reaction kettles in batches through a sodium hydroxide input passage b, simultaneously, stirrers 11 in the four reaction kettles 1 are started, after the sodium hydroxide is completely dissolved and reacts and the reaction temperature in the four reaction kettles 1 is not increased any more, a vacuum pump 2 arranged behind the four reaction kettles 1 is started, the measured methyl chloride is slowly introduced into the bottoms of the four reaction kettles 1 through a methyl chloride input passage c, the reaction is started until the reaction is finished, a reaction crude product is discharged into a settling tank 3 through a reaction liquid output passage e, after standing for a certain time, supernatant in the settling tank 3 is conveyed to a pre-fractionating tower 4 by a pump for fractionating, solid waste sodium chloride is discharged from the bottom of the settling tank 3, materials at the top of the pre-fractionating tower 4 are conveyed to a dehydrating tower 5 by a pump after being condensed, the method comprises the following steps of conveying materials in a tower kettle of a pre-separation tower 4 to a solvent recovery tower 7 by a pump for continuous rectification, extracting wastewater from the top of the solvent recovery tower 7, recycling excessive diethylene glycol monomethyl ether in the tower kettle of the solvent recovery tower 7 to four reaction kettles 1, continuously rectifying condensate by a dehydration tower 5, extracting wastewater from the top of the dehydration tower 5, conveying the materials in the tower kettle of the dehydration tower 5 to a finished product tower 6 by the pump for rectification again, extracting finished product diethylene glycol dimethyl ether from the top of the finished product tower 6, and remaining a small amount of residual liquid in the tower kettle of the finished product tower 6, wherein the wastewater and the residual liquid are conveyed to a waste treatment system for.
Wherein, the vacuum pump 2 is used for vacuumizing the reaction kettle 1, so that the chloromethane gas is slowly sent to the bottom of the reaction kettle 1, and the unreacted chloromethane gas is pumped away.
Preferably, the chemical reaction in the reaction vessel 1 is as follows:
reacting CH3OCH2CH2OCH2CH2OH and NaOH = CH3OCH2CH2OCH2CH2ONa + H2O with diethylene glycol monomethyl ether and sodium hydroxide to generate diethylene glycol monomethyl ether sodium and water;
CH3OCH2CH2OCH2CH2ONa + CH3Cl = CH3OCH2CH2OCH2CH2OCH3+ NaCl ↓, diethylene glycol methyl ether sodium and methyl chloride react to generate diethylene glycol dimethyl ether and sodium chloride solid;
preferably, the side wall of the reaction kettle 1 is provided with a transparent window 10, the turbidity change of the reaction liquid in the reaction kettle 1 is regularly observed through the transparent window 10, and the reaction in the reaction kettle 1 is judged to be finished when the turbidity of the reaction liquid is observed to be basically not changed any more, so that the observation method is visual and simple.
Further preferably, the lateral wall of reation kettle 1 is equipped with the spotlight 8 that highly match transparent window 10 set up apart from the position department of transparent window 10 keep a definite distance, spotlight 8's lamp holder sets up towards transparent window 10, be equipped with the photodiode array 9 of aiming at spotlight 8 lamp holder setting on transparent window 10, the light path between spotlight 8 and the photodiode array 9 and the setting of other parts mutually noninterfere that sets up in reation kettle 1, the photocurrent that detects when photodiode array 9 basically no longer changes judges for the reaction finishes in reation kettle 1, rely on the photocurrent that produces after the light that spotlight 8 sent is received to photodiode array 9 to judge, judge accurately.
Preferably, the reaction kettle 1 is a batch reaction kettle, and the working state of the reaction kettle 1 is T = 25-50 ℃ and P = -0.1-0.6 MPa.
Preferably, the settling tank 3 is an intermittent settling tank, and the working state of the settling tank 3 is T = 25-50 ℃ and P = 0-0.6 MPa.
Preferably, the pre-separation tower 4, the dehydration tower 5, the finished product tower 6 and the dissolution recovery tower 7 adopt rectification towers, the rectification conditions of the pre-separation tower 4 are T = 75-110 ℃, P = -0.1-0.2 MPa, the rectification conditions of the dehydration tower 5 are T = 80-100 ℃, P = -0.1-0.2 MPa, the rectification conditions of the finished product tower are T = 85-100 ℃, P = -0.1-0.2 MPa, the rectification conditions of the solvent recovery tower are T = 100-130 ℃, and P = -0.1-0.2 MPa.
Finally, it should be noted that the above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same, and although the present invention is described in detail with reference to the above-mentioned embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the specific embodiments of the present invention without departing from the spirit and scope of the present invention, and all the modifications or equivalent substitutions should be covered in the claims of the present invention.
Claims (7)
1. A production method of diethylene glycol dimethyl ether is characterized in that: the device comprises four reaction kettles, a settling tank, a pre-separation tower, a dehydration tower, a finished product tower and a solvent recovery tower which are arranged in parallel, wherein the single settling capacity of the settling tank is matched with that of the four reaction kettles, the upper end surfaces of the four reaction kettles are respectively provided with a common diethylene glycol methyl ether input passage, a sodium hydroxide input passage and an excess diethylene glycol methyl ether recycling passage, and the lower end surfaces of the four reaction kettles are respectively provided with a common methyl chloride input passage and a reaction liquid output passage; firstly, conveying a certain amount of diethylene glycol methyl ether into four reaction kettles by a pump through a diethylene glycol methyl ether input passage, then putting a certain amount of sodium hydroxide into the four reaction kettles in batches through a sodium hydroxide input passage, simultaneously starting stirrers of the four reaction kettles, starting a vacuum pump arranged behind the four reaction kettles after the sodium hydroxide is completely dissolved and reacted and the reaction temperature in the four reaction kettles is not increased, slowly introducing measured methyl chloride into the bottoms of the four reaction kettles through a methyl chloride input passage, starting reaction until the reaction is finished, discharging a reaction crude product into a settling tank through a reaction liquid output passage, standing for a certain time, conveying a supernatant in the settling tank to a pre-separation tower by the pump for rectification, discharging solid waste sodium chloride from the bottom of the settling tank, conveying a material at the top of the pre-separation tower to a dehydration tower by the pump after condensation, conveying a material in the kettle of the tower to a solvent recovery tower by the pump for continuous rectification, the method comprises the following steps of collecting waste water from the top of a solvent recovery tower, recycling excessive diethylene glycol monomethyl ether in tower bottom materials of the solvent recovery tower into four reaction kettles, continuously rectifying condensate by a dehydration tower, collecting waste water from the top of the dehydration tower, conveying the tower bottom materials of the dehydration tower to a finished product tower by a pump for rectification, collecting finished diethylene glycol dimethyl ether from the top of the finished product tower, and conveying a small amount of residual liquid to a finished product tower bottom, wherein the waste water and the residual liquid are conveyed to a waste treatment system for treatment.
2. The method for producing diethylene glycol dimethyl ether according to claim 1, characterized in that: the chemical reaction in the reaction kettle is as follows:
CH3OCH2CH2OCH2CH2OH+NaOH=CH3OCH2CH2OCH2CH2ONa+H2O；
CH3OCH2CH2OCH2CH2ONa+CH3Cl=CH3OCH2CH2OCH2CH2OCH3+NaCl↓。
3. the method for producing diethylene glycol dimethyl ether according to claim 1, characterized in that: the side wall of the reaction kettle is provided with a transparent window, the turbidity change of the reaction liquid in the reaction kettle is regularly observed through the transparent window, and the reaction in the reaction kettle is judged to be finished when the turbidity of the reaction liquid is basically not changed any more.
4. The method for producing diethylene glycol dimethyl ether according to claim 3, characterized in that: the lateral wall distance of reation kettle the position department of transparent window determining deviation is equipped with the altitude mixture match the spotlight that transparent window set up, the lamp holder orientation of spotlight transparent window sets up, be equipped with on the transparent window and aim at the photodiode array that the spotlight lamp holder set up, the spotlight with light path between the photodiode array with the setting of other parts mutually noninterferes that sets up in the reation kettle, work as the photocurrent that the photodiode array detected is judged to be the reation kettle in the end of reaction when no longer changing basically.
5. The method for producing diethylene glycol dimethyl ether according to claim 1, characterized in that: the reaction kettle adopts an intermittent reaction kettle, and the working state of the reaction kettle is T = 25-50 ℃, and P = -0.1-0.6 MPa.
6. The method for producing diethylene glycol dimethyl ether according to claim 1, characterized in that: the settling tank adopts an intermittent settling tank, and the working state of the settling tank is T = 25-50 ℃ and P = 0-0.6 MPa.
7. The method for producing diethylene glycol dimethyl ether according to claim 1, characterized in that: the pre-separation tower, the dehydration tower, the finished product tower and the dissolution recovery tower adopt rectification towers, the rectification conditions of the pre-separation tower are T = 75-110 ℃ and P = -0.1-0.2 MPa, the rectification conditions of the dehydration tower are T = 80-100 ℃ and P = -0.1-0.2 MPa, the rectification conditions of the finished product tower are T = 85-100 ℃ and P = -0.1-0.2 MPa, and the rectification conditions of the solvent recovery tower are T = 100-130 ℃ and P = -0.1-0.2 MPa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919415A (en) * | 2021-04-21 | 2021-06-08 | 沧州华宇特种气体科技有限公司 | Recovery method and recovery device of solvent for synthesizing diborane |
| CN114534288A (en) * | 2022-02-22 | 2022-05-27 | 沧州华宇特种气体科技有限公司 | Separation and solvent recovery method for salt-containing mixed solution |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1081666A (en) * | 1992-07-30 | 1994-02-09 | 杭州市化工研究所 | The production method of Polyethylene glycol dimethyl ether |
| CN104892371A (en) * | 2015-05-14 | 2015-09-09 | 安徽千和新材料科技发展有限公司 | Method for producing glycol dimethyl ether |
| CN106748669A (en) * | 2016-11-17 | 2017-05-31 | 安徽立兴化工有限公司 | A kind of method for synthesizing DPG ethyl methyl ether |
| CN107141201A (en) * | 2017-06-12 | 2017-09-08 | 沈阳化工大学 | A kind of method that glycol monoethyl ether prepares diethylene glycol dimethyl ether |
| CN110183313A (en) * | 2019-06-27 | 2019-08-30 | 河北迈太特化工有限公司 | A kind of preparation method of diethylene glycol dimethyl ether |
-
2021
- 2021-01-13 CN CN202110039909.8A patent/CN112624910A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1081666A (en) * | 1992-07-30 | 1994-02-09 | 杭州市化工研究所 | The production method of Polyethylene glycol dimethyl ether |
| CN104892371A (en) * | 2015-05-14 | 2015-09-09 | 安徽千和新材料科技发展有限公司 | Method for producing glycol dimethyl ether |
| CN106748669A (en) * | 2016-11-17 | 2017-05-31 | 安徽立兴化工有限公司 | A kind of method for synthesizing DPG ethyl methyl ether |
| CN107141201A (en) * | 2017-06-12 | 2017-09-08 | 沈阳化工大学 | A kind of method that glycol monoethyl ether prepares diethylene glycol dimethyl ether |
| CN110183313A (en) * | 2019-06-27 | 2019-08-30 | 河北迈太特化工有限公司 | A kind of preparation method of diethylene glycol dimethyl ether |
Non-Patent Citations (1)
| Title |
|---|
| 徐杰: "电子测量技术与应用第2版", 哈尔滨工业大学出版社, pages: 283 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112919415A (en) * | 2021-04-21 | 2021-06-08 | 沧州华宇特种气体科技有限公司 | Recovery method and recovery device of solvent for synthesizing diborane |
| CN114534288A (en) * | 2022-02-22 | 2022-05-27 | 沧州华宇特种气体科技有限公司 | Separation and solvent recovery method for salt-containing mixed solution |
| CN114534288B (en) * | 2022-02-22 | 2023-08-04 | 沧州华宇特种气体科技有限公司 | Separation and solvent recovery method of salt-containing mixed solution |
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