CN110790663B - Device and method for purifying neopentyl glycol byproduct sodium formate - Google Patents
Device and method for purifying neopentyl glycol byproduct sodium formate Download PDFInfo
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- CN110790663B CN110790663B CN201910940393.7A CN201910940393A CN110790663B CN 110790663 B CN110790663 B CN 110790663B CN 201910940393 A CN201910940393 A CN 201910940393A CN 110790663 B CN110790663 B CN 110790663B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/36—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions with formation of hydroxy groups, which may occur via intermediates being derivatives of hydroxy, e.g. O-metal
- C07C29/38—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions with formation of hydroxy groups, which may occur via intermediates being derivatives of hydroxy, e.g. O-metal by reaction with aldehydes or ketones
Abstract
The invention relates to a device and a method for purifying neopentyl glycol byproduct sodium formate, which comprises an isobutyraldehyde tank, a formaldehyde tank, a liquid alkali tank, a formic acid tank, a condensation kettle, a neutralization kettle, a distillation tower, a reduced pressure evaporator and a centrifugal machine, and is characterized in that a dealcoholization and dealdehyding tower, a normal pressure evaporator, a mother liquor tank and a secondary evaporator are additionally arranged; the neutralizing kettle is sequentially connected with the dealcoholization and aldehyde removal tower, the normal pressure evaporator, the reduced pressure evaporator, the centrifuge, the mother liquor tank and the secondary evaporator through pipelines, the other outlet of the normal pressure evaporator is connected with the distillation tower through a pipeline, the outlet of the distillation tower is connected to the secondary evaporator through a pipeline, the other outlet of the dealcoholization and aldehyde removal tower is connected to the condensation kettle through a pipeline, and the other outlet of the mother liquor tank is connected to the normal pressure evaporator through a pipeline. The invention has the advantages that: the purified sodium formate has pure color and smell, and the content is more than 96 percent; by adopting the device and the method to purify the sodium formate, the consumption of raw materials is reduced, and the consumption of steam is greatly reduced.
Description
Technical Field
The invention belongs to the technical field of chemical production, relates to the field of neopentyl glycol production, and particularly relates to a device and a method for purifying a neopentyl glycol byproduct sodium formate.
Background
Neopentyl glycol is a white crystalline solid, is odorless and hygroscopic, and is mainly used for producing unsaturated resins, polyester powder coatings, oil-free alkyd resins, polyurethane foam plastics, namely, plasticizers of elastomers, synthetic plasticizers, surfactants, insulating materials, printing inks, polymerization inhibitors, synthetic aviation lubricating oil additives and the like. In addition, the method is also applied to the pharmaceutical industry; meanwhile, neopentyl glycol is an excellent solvent and can be used for selective separation of aromatic hydrocarbon and naphthenic hydrocarbon.
The disproportionation production process of neopentyl glycol is characterized by using isobutyraldehyde and formaldehyde as raw materials, condensing at 30-35 ℃ and with the pH value of 9-11 and the presence of an alkali catalyst to generate hydroxyl tert-butyraldehyde, then reducing the hydroxyl tert-butyraldehyde and excessive formaldehyde under the strong alkali condition to obtain neopentyl glycol, oxidizing the formaldehyde, and neutralizing the formaldehyde with liquid alkali to generate sodium formate; the reaction liquid is firstly neutralized by formic acid, and then concentrated, lightness removed and rectified to obtain the finished product of neopentyl glycol after alcohol and salt separation by reduced pressure evaporation.
The by-product sodium formate produced by the disproportionation method is yellow or brown crystal in appearance, has formic acid smell, is low in purity and contains 86-90% of sodium formate, and still contains a small amount of neopentyl glycol.
Disclosure of Invention
The invention aims to overcome the defects that the purity of the byproduct sodium formate in the production of neopentyl glycol is not high, the color is yellow or brown, and the byproduct sodium formate has formic acid smell and the like, and provides a device and a method for purifying the byproduct sodium formate of neopentyl glycol.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a neopentyl glycol by-product sodium formate's purification device includes current following equipment: isobutyraldehyde groove, formaldehyde groove, liquid caustic soda groove, formic acid groove, condensation kettle, neutralization kettle, distillation column, decompression evaporator, centrifuge, its characterized in that newly increases following equipment: a dealcoholization and aldehyde removal tower, a normal pressure evaporator, a mother liquor tank and a secondary evaporator;
the other outlet of the atmospheric evaporator is connected with the distillation tower through a pipeline, the outlet of the distillation tower is connected to the secondary evaporator, the other outlet of the dealcoholization and dealdehyding tower is connected to the condensation kettle through a pipeline, and the other outlet of the mother liquid tank is connected to the atmospheric evaporator through a pipeline.
A method for purifying neopentyl glycol byproduct sodium formate is characterized by comprising the following steps:
(1) according to the mass ratio of isobutyraldehyde, formaldehyde and liquid caustic soda of 0.75: 1.70: 1.33 delivering isobutyraldehyde, formaldehyde and a liquid alkali catalyst (NaOH 32%) into a condensation kettle for reaction, controlling the temperature to be 35-40 ℃ and the pH value to be 9-11, delivering the reaction liquid into a neutralization kettle after 4 hours of reaction, heating the neutralization kettle to 55 ℃ first, then heating the neutralization kettle to 60 ℃ again, adding formic acid into the neutralization kettle within 30min after the temperature rise is finished for neutralization for 22-40min, and controlling the pH to be 7.0-7.5;
(2) the neutralized reaction liquid enters a dealcoholization and dealdehyding tower to remove a small amount of methanol and formaldehyde, the temperature of the dealcoholization and dealdehyding tower is controlled to be 82-85 ℃, the time is 10-20min, and the dilute formaldehyde is condensed and then returns to a condensation kettle to react;
(3) dehydrating the solution after dealcoholization and dealdehydization in a normal pressure evaporator at the temperature of 102 ℃ and the temperature of 105 ℃ for 30-60min, evaporating to form a salt phase and an alcohol phase, rectifying the alcohol phase in a distillation tower, evaporating the salt phase in a reduced pressure evaporator again at the temperature of 65-70 ℃, the temperature of 0.080 MPa to-0.090 MPa for 30-40min, centrifuging the evaporated concentrated solution in a centrifuge to obtain wet sodium formate, centrifuging at the temperature of 700r/min for 3-5min, feeding the centrifuged mother solution in a mother solution tank, feeding the mother solution and high waste residues from the distillation tower into a secondary evaporator for evaporation, and controlling the temperature of 110 ℃ and 118 ℃, the pressure of-0.065 MPa to-0.070 MPa for 20-30 min;
(4) drying the centrifuged wet product sodium formate at the temperature of 145-155 ℃ for 10-20min to obtain the finished product sodium formate (the content is 96-98%).
The normal pressure evaporation extraction separation technology is adopted, the ingredients are prepared during the condensation reaction, the ingredient process water is saved, the reaction temperature is controlled by using a weak alkaline catalyst in the early stage of the reaction, and the dilute formaldehyde generated in the production is recycled during the ingredients, so that the utilization rate of isobutyraldehyde is improved, and the consumption of raw materials of isobutyraldehyde and formaldehyde is reduced to a certain extent; when the alkoxide is evaporated and separated under normal pressure, the temperature is controlled within 100 ℃, and the steam pressure is normally controlled to be 3.5Kg, so that the production requirement can be met, compared with the decompression evaporation operation of the prior art, the alkoxide separation in the production is influenced when the steam pressure is less than 6 Kg; the condensation reaction is firstly carried out with dealcoholization and dealdehyding, thereby preventing excessive oxidation color development and increase of side reactants, controlling the neopentyl glycol carried by salt phase within 1 percent, and effectively improving the purity and chromaticity requirements of sodium formate.
The invention has the advantages that:
1. the purified sodium formate has pure color and smell, and the content of the sodium formate is more than 96 percent; 2. the device and the method are adopted to purify the sodium formate, so that the consumption of raw materials is reduced, and especially the steam consumption is greatly reduced. According to the market quotation at present, the purified and modified sodium formate content of neopentyl glycol reaches 96-98%, the delivery price is more than 1200 Yuan/ton (90% of the content of sodium formate has large fluctuation in delivery grids, even 350-450 Yuan/ton can not be delivered), 10000-ton of 96-98% of sodium formate can be produced by using the existing production capacity of 15000 tons of neopentyl glycol per year, 800 ten thousand Yuan gross profit is created newly every year, the cost increased by technical improvement is deducted, and the pure profit can be increased by 600 Yuan.
Drawings
FIG. 1 is a schematic diagram of a process for purifying sodium formate as a by-product of neopentyl glycol.
Detailed Description
The invention is further illustrated with reference to fig. 1:
a neopentyl glycol by-product sodium formate's purification device includes following equipment: the isobutyraldehyde tank, the formaldehyde tank and the liquid caustic soda tank are respectively connected with a condensation kettle through pipelines, the condensation kettle is sequentially connected with a neutralization kettle, a dealcoholization and dealdehyding tower, an atmospheric pressure evaporator, a reduced pressure evaporator, a centrifuge, a mother liquor tank and a secondary evaporator through pipelines, the other outlet of the atmospheric pressure evaporator is connected with a distillation tower through a pipeline, the outlet of the distillation tower is connected with the secondary evaporator through a pipeline, the formaldehyde tank is connected with the neutralization kettle through a pipeline, the other outlet of the dealcoholization and dealdehyding tower is connected with the condensation kettle through a pipeline, and the other outlet of the mother liquor tank is connected with the atmospheric pressure evaporator through a pipeline.
A method for purifying neopentyl glycol byproduct sodium formate comprises the following specific implementation steps:
example 1
(1) Isobutyraldehyde 7.9Kg/L, formaldehyde 11.1Kg/L, liquid alkali catalyst (32% NaOH)13.55Kg/L is sent into a condensation kettle for reaction, the temperature and the pH value are controlled to be 40 ℃, the reaction liquid is sent into a neutralization kettle after 4 hours of reaction, the neutralization kettle is heated to 55 ℃ firstly and then heated to 60 ℃ again, formic acid is added into the neutralization kettle within 30min after the temperature rise for neutralization for 25min, and the pH value is controlled to be 7.0;
(2) the neutralized reaction liquid enters a dealcoholization and dealdehyding tower to remove a small amount of methanol and formaldehyde, the temperature of the dealcoholization and dealdehyding tower is controlled to be 85 ℃, the time is 15min, and the dilute formaldehyde is condensed and then returns to a condensation kettle to react;
(3) the solution after dealcoholization and dealdehydization enters a normal pressure evaporator to be dehydrated, the temperature is controlled to be 105 ℃ for 50min, a salt phase and an alcohol phase are formed after evaporation, the alcohol phase enters a distillation tower to be rectified, the salt phase enters a reduced pressure evaporator to be evaporated again, the temperature is controlled to be 70 ℃, the pressure is controlled to be-0.090 Mpa, the time is 35min, the evaporated concentrated solution enters a centrifugal machine to be centrifuged to obtain wet sodium formate, the wet sodium formate is centrifuged for 5min at 400r/min, the centrifuged mother solution enters a mother solution tank, the mother solution and high waste residues from the distillation tower are sent to a secondary generator to be evaporated, the temperature is controlled to be 118 ℃, the pressure is controlled to be-0.065 Mpa, and the time is 25 min;
(4) and drying the centrifuged wet sodium formate at 150 ℃ for 15min to obtain the finished sodium formate (the content is 96-98%).
Claims (2)
1. A neopentyl glycol by-product sodium formate's purification device includes current following equipment: isobutyraldehyde groove, formaldehyde groove, liquid caustic soda groove, formic acid groove, condensation kettle, neutralization kettle, distillation column, decompression evaporator, centrifuge, its characterized in that newly increases following equipment: a dealcoholization and aldehyde removal tower, a normal pressure evaporator, a mother liquor tank and a secondary evaporator;
the other outlet of the atmospheric evaporator is connected with the distillation tower through a pipeline, the outlet of the distillation tower is connected to the secondary evaporator, the other outlet of the dealcoholization and dealdehyding tower is connected to the condensation kettle through a pipeline, and the other outlet of the mother liquid tank is connected to the atmospheric evaporator through a pipeline.
2. A method for purifying neopentyl glycol byproduct sodium formate is characterized by comprising the following steps:
(1) according to the mass ratio of isobutyraldehyde, formaldehyde and liquid caustic soda of 0.75: 1.70: 1.33 delivering isobutyraldehyde, formaldehyde and liquid caustic soda into a condensation kettle for reaction, controlling the temperature to be 35-40 ℃ and the pH value to be 9-11, delivering the reaction liquid into a neutralization kettle after reacting for 4h, heating the neutralization kettle to 55 ℃ first, then heating to 60 ℃ again, adding formic acid into the neutralization kettle within 30min after heating for neutralization for 22-40min, and controlling the pH value to be 7.0-7.5;
(2) the neutralized reaction liquid enters a dealcoholization and dealdehyding tower to remove a small amount of methanol and formaldehyde, the temperature of the dealcoholization and dealdehyding tower is controlled to be 82-85 ℃, the time is 10-20min, and the dilute formaldehyde is condensed and then returns to a condensation kettle to react;
(3) dehydrating the solution after dealcoholization and dealdehydization in a normal pressure evaporator at the temperature of 102 ℃ and the temperature of 105 ℃ for 30-60min, evaporating to form a salt phase and an alcohol phase, rectifying the alcohol phase in a distillation tower, evaporating the salt phase in a reduced pressure evaporator again at the temperature of 65-70 ℃, controlling the temperature of 0.080 to-0.090 MPa for 30-40min, centrifuging the evaporated concentrated solution in a centrifuge to obtain wet sodium formate, centrifuging at the temperature of 700r/min for 3-5min at 400 ℃, feeding the centrifuged mother solution in a mother solution tank, feeding the mother solution and high waste residues from the distillation tower into a secondary evaporator for evaporation, and controlling the temperature of 118 ℃ at 110 ℃ and the pressure of-0.065 to-0.070 MPa for 20-30 min;
(4) drying the centrifuged wet product sodium formate at 155 ℃ of 145-155 ℃ for 10-20min to obtain the finished product sodium formate.
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| CN101591221A (en) * | 2009-06-08 | 2009-12-02 | 无锡百川化工股份有限公司 | A kind of low temperature condensation and condensated liquid carried out pretreated method |
| CN104672059A (en) * | 2015-02-04 | 2015-06-03 | 沾化瑜凯新材料科技有限公司 | Production method of neopentyl glycol |
| CN105503573A (en) * | 2015-12-23 | 2016-04-20 | 安徽金禾实业股份有限公司 | Method and device for separation treatment of sodium formate in NPG (neopentyl glycol) production technology |
| CN105541556A (en) * | 2016-02-23 | 2016-05-04 | 山东省化工研究院 | Neopentyl glycol and sodium formate separating method |
| CN109824477A (en) * | 2019-02-28 | 2019-05-31 | 东营市科维生物技术有限公司 | Neopentyl glycol and its alkaline process preparation method and application |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591221A (en) * | 2009-06-08 | 2009-12-02 | 无锡百川化工股份有限公司 | A kind of low temperature condensation and condensated liquid carried out pretreated method |
| CN104672059A (en) * | 2015-02-04 | 2015-06-03 | 沾化瑜凯新材料科技有限公司 | Production method of neopentyl glycol |
| CN105503573A (en) * | 2015-12-23 | 2016-04-20 | 安徽金禾实业股份有限公司 | Method and device for separation treatment of sodium formate in NPG (neopentyl glycol) production technology |
| CN105541556A (en) * | 2016-02-23 | 2016-05-04 | 山东省化工研究院 | Neopentyl glycol and sodium formate separating method |
| CN109824477A (en) * | 2019-02-28 | 2019-05-31 | 东营市科维生物技术有限公司 | Neopentyl glycol and its alkaline process preparation method and application |
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