CN114539038A - Preparation method of propylene glycol monobutyl ether - Google Patents

Preparation method of propylene glycol monobutyl ether Download PDF

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Publication number
CN114539038A
CN114539038A CN202210267391.8A CN202210267391A CN114539038A CN 114539038 A CN114539038 A CN 114539038A CN 202210267391 A CN202210267391 A CN 202210267391A CN 114539038 A CN114539038 A CN 114539038A
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Prior art keywords
propylene glycol
monobutyl ether
glycol monobutyl
furnace body
furnace
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CN202210267391.8A
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Chinese (zh)
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胡斌
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Nanjing Jiayan New Material Technology Co ltd
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Nanjing Jiayan New Material Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/01Preparation of ethers
    • C07C41/02Preparation of ethers from oxiranes
    • C07C41/03Preparation of ethers from oxiranes by reaction of oxirane rings with hydroxy groups
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/18Absorbing units; Liquid distributors therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/06Halogens; Compounds thereof
    • B01J27/08Halides
    • B01J27/12Fluorides

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a preparation method of propylene glycol monobutyl ether, belonging to the technical field of preparation of propylene glycol monobutyl ether and comprising the following steps: a01: preparing a magnesium salt solution by magnesium chloride and deionized water, dissolving precipitator sodium hydroxide and sodium carbonate by the deionized water, and mixing the precipitator sodium hydroxide and the sodium carbonate with the prepared magnesium salt solution; a02: stirring vigorously for reaction, aging at 70 deg.C for several hours, filtering out precipitate, placing in a muffle furnace for high temperature roasting to obtain carrier MgO, drying to constant mass, placing in a muffle furnace for high temperature roasting at 600 deg.C to obtain solid base catalyst KF/MgO; a03: adding solid base catalyst and N-butanol into a high-pressure reaction kettle, and adding N2Replacing air in the kettle; a04: after the temperature of the reaction kettle reaches the temperature, the reaction kettle startsCooling and discharging, and fractionating to obtain the finished product of the propylene glycol butyl ether. The invention uses the solid base catalyst KF/MgO to catalyze the propylene oxide and the butanol to synthesize the propylene glycol butyl ether, is a green synthesis process, and has great significance for environmental protection.

Description

Preparation method of propylene glycol monobutyl ether
Technical Field
The invention relates to the technical field of preparation of propylene glycol monobutyl ether, in particular to a preparation method of propylene glycol monobutyl ether.
Background
Propylene glycol ether is a low-toxicity excellent solvent prepared by the reaction of propylene oxide and low-carbon alcohol, the propylene glycol ether mainly comprises propylene glycol methyl ether (PM), propylene glycol ethyl ether (PE), propylene glycol butyl ether (PB) and the like and corresponding esters thereof, the toxicity of the propylene glycol ether is far lower than that of ethylene glycol ethers due to the unique chemical structure with double functions of hydrophily and lipophilicity, and the propylene glycol ether is an excellent general solvent, so the propylene glycol ether product is gradually substituted for the ethylene glycol ethers and is widely used in the industries of coatings, printing, dyes, printing inks, leather, electronic chemicals, PS (polystyrene) plate cleaning, photosensitive adhesives, synthetic brake fluids, jet fuel additives and the like, the propylene glycol ether is used as an important organic raw material and a high-grade organic solvent for fine chemical reaction due to the low toxicity, safety and other excellent performances, in recent years, the rapid development is abroad, on the contrary, the ethylene glycol ether has the killing power on human bodies, if the toxicity is greater, the deformity and the erythrocyte are dissolved, and the damage to the bone development is caused;
at present, the traditional propylene glycol monobutyl ether is synthesized by generally adopting a homogeneous catalysis process, so that the problems of easy corrosion of equipment and difficult separation of a catalyst and a product exist, the used related catalyst is not environment-friendly enough, and related materials can generate peculiar smell to be accumulated in a furnace when being roasted at high temperature, and the peculiar smell can be paved when a user opens a furnace door, so that the experience is very poor.
Disclosure of Invention
The present invention is to solve the above problems and to provide a process for producing propylene glycol monobutyl ether.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of propylene glycol monobutyl ether comprises the following steps:
the method comprises the following steps:
a01: preparing a magnesium salt solution by magnesium chloride and deionized water, dissolving precipitator sodium hydroxide and sodium carbonate by the deionized water, and mixing the precipitator sodium hydroxide and the sodium carbonate with the prepared magnesium salt solution;
a02: stirring vigorously for reaction, aging at 70 deg.C for several hours, filtering out precipitate, drying to constant mass, placing in muffle furnace, high temperature roasting to obtain carrier MgO, mixing 30% load KF and carrier MgO by solid phase grinding method, drying to constant mass, placing in muffle furnace, high temperature roasting at 600 deg.C to obtain solid base catalyst KF/MgO;
A03:adding solid base catalyst and N-butanol into a 4L high-pressure reaction kettle2Replacing the air in the kettle for 3 times;
a04: and (3) slowly introducing propylene oxide after the temperature of the reaction kettle reaches the set temperature, controlling the pressure in the kettle to be 0.2-0.5 MPa, continuously maintaining the pressure at the set temperature for reaction after the introduction of the propylene oxide is finished until the pressure in the kettle is kept unchanged within 30 min, starting cooling and discharging to obtain a propylene glycol butyl ether crude product, and fractionating to obtain a propylene glycol butyl ether finished product.
Further characterized in that the muffle furnace consists of a furnace body, a controller and a purifying device.
The furnace body is characterized in that the controller is arranged on the upper end surface of the furnace body, the controller comprises an indicator light, a display, an ammeter and a switch, and the controller is connected with the furnace body through a connecting wire.
The furnace body is characterized in that a furnace door is rotatably connected to the surface of the front end of the furnace body, a mounting seat is fixedly mounted on one side of the furnace door, a door handle is elastically mounted in the mounting seat, and a lock pin is arranged on the surface of the door handle.
Further, a hearth is arranged on the surface of the front end of the furnace body, an air passage is further arranged in the furnace body and communicated with the hearth, the tail end of the air passage is connected with an electronic valve, and the tail end of the electronic valve is connected with a purification device.
Further, purifier includes rose box, division board, ventilation fan, blast pipe, the fixed intermediate position department that sets up in the rose box of division board, the ventilation fan sets up the one side at the division board, the blast pipe sets up the one end at the rose box, and blast pipe and rose box intercommunication.
Further, the front end of the furnace body is also fixedly provided with a locking ring, the locking ring is positioned at one side of the hearth opening, and the locking opening on the locking ring is matched with the lock pin
Further, four bearing legs are fixedly arranged at the lower end of the furnace body.
Compared with the prior art, the invention has the following beneficial effects:
(1) the solid base catalyst KF/MgO is an environment-friendly solid base catalyst with higher catalytic activity, has the advantages of mild reaction conditions, high catalytic activity, easy separation from products, recyclable catalyst and the like, and is a green synthesis process for catalyzing epoxypropane and butanol to synthesize propylene glycol butyl ether by using the solid base catalyst KF/MgO, can be applied to actual production and has great significance for environmental protection.
(2) When carrying out the calcination operation to the material, electronic valve is in the closed condition, avoid the heat outflow, the material calcination is accomplished the back, open electronic valve and ventilation fan, the ventilation fan passes through the air duct, electronic valve inhales gas to the rose box in, the pure water is filled to one side that is located the partition plate in the rose box, the air is utilizing the blast pipe to discharge after inhaling through the pure water, thereby play the effect of purification, can effectively solve the peculiar smell and pile up in the stove, when the user opens the furnace gate, the peculiar smell can shop front the problem that comes.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention;
FIG. 2 is a schematic view of the overall structure of the muffle furnace of the present invention;
FIG. 3 is a schematic view of the connection between the furnace body and the filter box according to the present invention;
FIG. 4 is a schematic view of the door handle of the present invention.
In the figure: 1. a furnace body; 2. a load bearing foot; 3. a locking ring; 4. a furnace door; 5. a door handle; 6. a mounting seat; 7. a hearth; 8. a lock pin; 9. a spring; 10. a controller; 11. an indicator light; 12. a display; 13. an ammeter; 14. a switch; 15. a device housing; 16. an exhaust pipe; 17. an air duct; 18. an electronic valve; 19. a filter box; 20. a partition plate; 21. ventilating fan.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
As shown in fig. 1, a preparation method of propylene glycol monobutyl ether comprises the following steps:
a01: preparing a magnesium salt solution by magnesium chloride and deionized water, dissolving precipitator sodium hydroxide and sodium carbonate by the deionized water, and mixing the precipitator sodium hydroxide and the sodium carbonate with the prepared magnesium salt solution;
a02: stirring vigorously for reaction, aging at 70 deg.C for several hours, filtering out precipitate, drying to constant mass, placing in muffle furnace, high temperature roasting to obtain carrier MgO, mixing 30% load KF and carrier MgO by solid phase grinding method, drying to constant mass, placing in muffle furnace, high temperature roasting at 600 deg.C to obtain solid base catalyst KF/MgO;
a03: adding solid base catalyst and N-butanol into a 4L high-pressure reaction kettle2Replacing the air in the kettle for 3 times;
a04: slowly introducing propylene oxide after the temperature of the reaction kettle reaches a set temperature, controlling the pressure in the kettle to be 0.2-0.5 MPa, continuously maintaining the pressure at the set temperature for reaction after the propylene oxide introduction is finished until the pressure in the kettle is kept unchanged within 30 min, starting cooling and discharging to obtain a propylene glycol butyl ether crude product, and fractionating to obtain a propylene glycol butyl ether finished product;
the prepared solid base catalyst is mainly characterized in that butanol is activated to form alkoxy negative ions, the activated butanol reacts with propylene oxide to generate propylene glycol butyl ether, the molecular structure of the propylene oxide is asymmetric, after ring opening, the alkoxy negative ions formed by butanol activation can be respectively combined with primary carbon and secondary carbon to generate two propylene glycol butyl ether isomers, primary ether is mainly generated by base catalysis, and the propylene glycol butyl ether obtained by reaction can continuously react with the propylene oxide to generate polypropylene glycol ethers such as dipropylene glycol butyl ether and the like.
As shown in fig. 2-4, the muffle furnace is composed of a furnace body 1, a controller 10 and a purification device, the controller 10 is arranged on the upper end surface of the furnace body 1, the controller 10 comprises an indicator lamp 11, a display 12, an ammeter 13 and a switch 14, the controller 10 is connected with the furnace body 1 through a connecting wire, the furnace body is used for roasting raw materials, the controller 10 is used for controlling the opening of the furnace body, and the purification device is used for purifying gas in the furnace body;
the front end surface of the furnace body 1 is rotatably connected with a furnace door 4, one side of the furnace door 4 is fixedly provided with a mounting seat 6, a door handle 5 is elastically installed in the mounting seat 6, the surface of the door handle 5 is provided with a lock pin 8, the front end of the furnace body 1 is also fixedly provided with a lock ring 3, the lock ring 3 is positioned at one side of a hearth opening of a furnace 7, the lock opening on the lock ring 3 is matched with the lock pin 8, when leftward pressure is applied to the door handle 5, a spring 9 positioned at one side of the door handle 5 contracts and deforms, so that the lock pin 8 can be separated from the lock ring 3, the furnace door 4 is opened, a heated object is placed into the furnace 7, then the furnace door 4 is closed, the acting force on the door handle 5 is relieved, and the lock pin 8 positioned on the door handle 5 is bounced into the lock ring 3 again under the influence of the spring 9;
the front end surface of the furnace body 1 is provided with a hearth 7, the interior of the furnace body 1 is also provided with an air duct 17, the air duct 17 is communicated with the hearth 7, the tail end of the air duct 17 is connected with an electronic valve 18, the tail end of the electronic valve 18 is connected with a purification device, the purification device comprises a filter box 19, a partition plate 20, an air fan 21 and an exhaust pipe 16, the partition plate 20 is fixedly arranged at the middle position in the filter box 19, the air fan 21 is arranged at one side of the partition plate 20, the exhaust pipe 16 is arranged at one end of the filter box 19, and the exhaust pipe 16 is communicated with the filter box 19;
during specific work, when the material is roasted, the electronic valve 18 is in a closed state, heat outflow is avoided, after roasting of the material is completed, the electronic valve 18 and the ventilation fan 21 are opened, the ventilation fan 21 sucks gas into the filter box 19 through the air duct 17 and the electronic valve 18, one side of the partition plate 20 in the filter box 19 is filled with purified water, and the air is exhausted by the exhaust pipe 16 after passing through the purified water after being sucked, so that the purification effect is achieved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (8)

1. The preparation method of the propylene glycol monobutyl ether is characterized by comprising the following steps:
a01: preparing a magnesium salt solution by using magnesium chloride and deionized water, dissolving precipitator sodium hydroxide and sodium carbonate by using the deionized water, and mixing the solution with the prepared magnesium salt solution;
a02: stirring vigorously for reaction, aging at 70 deg.C for several hours, filtering out precipitate, drying to constant mass, placing in muffle furnace, high temperature roasting to obtain carrier MgO, mixing 30% load KF and carrier MgO by solid phase grinding method, drying to constant mass, placing in muffle furnace, high temperature roasting at 600 deg.C to obtain solid base catalyst KF/MgO;
a03: adding solid base catalyst and N-butanol into a 4L high-pressure reaction kettle2Replacing the air in the kettle for 3 times;
a04: and (3) slowly introducing propylene oxide after the temperature of the reaction kettle reaches the set temperature, controlling the pressure in the kettle to be 0.2-0.5 MPa, continuously maintaining the pressure at the set temperature for reaction after the introduction of the propylene oxide is finished until the pressure in the kettle is kept unchanged within 30 min, starting cooling and discharging to obtain a propylene glycol butyl ether crude product, and fractionating to obtain a propylene glycol butyl ether finished product.
2. The process according to claim 1, wherein the propylene glycol monobutyl ether is prepared by: the muffle furnace consists of a furnace body (1), a controller (10) and a purifying device.
3. The process according to claim 2, wherein the propylene glycol monobutyl ether is prepared by: the furnace body (1) is arranged on the upper end surface of the furnace body (10), the controller (10) comprises an indicator lamp (11), a display (12), an ammeter (13) and a switch (14), and the controller (10) is connected with the furnace body (1) through a connecting line.
4. The process according to claim 3, wherein the propylene glycol monobutyl ether is prepared by: the front end surface of the furnace body (1) is rotatably connected with a furnace door (4), a mounting seat (6) is fixedly mounted on one side of the furnace door (4), a door handle (5) is elastically mounted in the mounting seat (6), and a lock pin (8) is arranged on the surface of the door handle (5).
5. The process according to claim 4, wherein the propylene glycol monobutyl ether is prepared by: furnace (7) have been seted up on the front end surface of furnace body (1), still be provided with air duct (17) in furnace body (1), air duct (17) and furnace (7) intercommunication, and the end-to-end connection of air duct (17) has electronic valve (18), the end-to-end connection of electronic valve (18) has purifier.
6. The process according to claim 2, wherein the propylene glycol monobutyl ether is prepared by: purifier includes rose box (19), division board (20), ventilates fan (21), blast pipe (16), division board (20) are fixed to be set up the intermediate position department in rose box (19), ventilate fan (21) sets up the one side at division board (20), blast pipe (16) set up the one end at rose box (19), and blast pipe (16) and rose box (19) intercommunication.
7. The process according to claim 2, wherein the propylene glycol monobutyl ether is prepared by: the front end of the furnace body (1) is also fixedly provided with a locking ring (3), the locking ring (3) is positioned at one side of the hearth opening of the hearth (7), and the locking opening on the locking ring (3) is matched with the locking pin (8).
8. The process according to claim 2, wherein the propylene glycol monobutyl ether is prepared by: the lower end of the furnace body (1) is fixedly provided with four bearing legs (2).
CN202210267391.8A 2022-03-17 2022-03-17 Preparation method of propylene glycol monobutyl ether Pending CN114539038A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107328231A (en) * 2017-09-04 2017-11-07 钦州学院 A kind of Muffle furnace apparatus of environmental protection
CN107602354A (en) * 2017-09-15 2018-01-19 常州大学 A kind of method of synthesizing propanediol butyl ether
CN211823773U (en) * 2020-01-09 2020-10-30 甘肃奥科检测有限公司 Muffle furnace with smoke exhaust and purification treatment function
CN215002848U (en) * 2021-04-28 2021-12-03 成都栩哲医药科技有限公司 Environment-friendly muffle furnace
CN215002849U (en) * 2021-04-28 2021-12-03 成都栩哲医药科技有限公司 Muffle furnace

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107328231A (en) * 2017-09-04 2017-11-07 钦州学院 A kind of Muffle furnace apparatus of environmental protection
CN107602354A (en) * 2017-09-15 2018-01-19 常州大学 A kind of method of synthesizing propanediol butyl ether
CN211823773U (en) * 2020-01-09 2020-10-30 甘肃奥科检测有限公司 Muffle furnace with smoke exhaust and purification treatment function
CN215002848U (en) * 2021-04-28 2021-12-03 成都栩哲医药科技有限公司 Environment-friendly muffle furnace
CN215002849U (en) * 2021-04-28 2021-12-03 成都栩哲医药科技有限公司 Muffle furnace

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
宋文娟等: "固体碱催化剂KF/MgO催化合成丙二醇丁醚的绿色工艺研究", 涂料工业, vol. 48, no. 5, pages 34 *
郭登峰;刘红;刘准;曹惠庆;赵文;石兆君;: "固体碱催化剂KF/Al_2O_3催化合成乙二醇丁醚", 南京理工大学学报(自然科学版), no. 01, pages 122 - 126 *

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Application publication date: 20220527