CN114315517A - Production method of low-energy-consumption 98-grade pentaerythritol - Google Patents
Production method of low-energy-consumption 98-grade pentaerythritol Download PDFInfo
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- CN114315517A CN114315517A CN202111683565.0A CN202111683565A CN114315517A CN 114315517 A CN114315517 A CN 114315517A CN 202111683565 A CN202111683565 A CN 202111683565A CN 114315517 A CN114315517 A CN 114315517A
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- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 36
- 238000005265 energy consumption Methods 0.000 title claims abstract description 26
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 81
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000002425 crystallisation Methods 0.000 claims abstract description 30
- 230000008025 crystallization Effects 0.000 claims abstract description 30
- 239000007788 liquid Substances 0.000 claims abstract description 30
- 230000007062 hydrolysis Effects 0.000 claims abstract description 24
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 24
- 238000005406 washing Methods 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000001704 evaporation Methods 0.000 claims abstract description 19
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 claims abstract description 18
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 18
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000019253 formic acid Nutrition 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 230000008020 evaporation Effects 0.000 claims abstract description 13
- 238000006482 condensation reaction Methods 0.000 claims abstract description 11
- 238000004806 packaging method and process Methods 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 15
- 239000002245 particle Substances 0.000 claims description 15
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 8
- 238000009835 boiling Methods 0.000 claims description 7
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000007873 sieving Methods 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 3
- 238000012858 packaging process Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 2
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 229910052708 sodium Inorganic materials 0.000 abstract description 2
- 239000011734 sodium Substances 0.000 abstract description 2
- 238000010979 pH adjustment Methods 0.000 abstract 1
- 229940059574 pentaerithrityl Drugs 0.000 description 25
- 239000003973 paint Substances 0.000 description 6
- 239000008187 granular material Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920000180 alkyd Polymers 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
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- 239000003063 flame retardant Substances 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- 239000004114 Ammonium polyphosphate Substances 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- -1 Fatty acid esters Chemical class 0.000 description 1
- TZRXHJWUDPFEEY-UHFFFAOYSA-N Pentaerythritol Tetranitrate Chemical compound [O-][N+](=O)OCC(CO[N+]([O-])=O)(CO[N+]([O-])=O)CO[N+]([O-])=O TZRXHJWUDPFEEY-UHFFFAOYSA-N 0.000 description 1
- 239000000026 Pentaerythritol tetranitrate Substances 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 description 1
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 description 1
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 description 1
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 1
- 229920001276 ammonium polyphosphate Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
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- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 229960004321 pentaerithrityl tetranitrate Drugs 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
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- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a production method of 98-grade pentaerythritol with low energy consumption, which comprises 8 steps of condensation reaction, formaldehyde removal and pH adjustment, hydrolysis, evaporation, crystallization, separation, washing, drying and packaging and the like in sequence. The invention adopts a sodium method to intermittently produce pentaerythritol, wherein the pentaerythritol takes formaldehyde and acetaldehyde as raw materials to carry out condensation reaction under the catalysis of liquid alkali, hydrogen peroxide is used to remove residual formaldehyde when the reaction is stopped, formic acid is used to adjust the PH to about 5, and then 98-grade pentaerythritol finished products are obtained through the working procedures of high-temperature high-pressure hydrolysis, efficient and continuous MVR evaporation, crystallization, separation, washing, drying, packaging and the like. The method can realize the production of 98-grade pentaerythritol with low energy consumption and reduce the generation of byproducts, thereby improving the yield, ensuring that the removal rate of formaldehyde reaches 100 percent and removing the residual formaldehyde in the product. Only a small amount of steam is used in the evaporation process, and the investment of production cost is greatly reduced.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a production method of low-energy-consumption 98-grade pentaerythritol.
Background
Pentaerythritol, white crystals or powder, is flammable, is easy to be esterified by common organic acid, and is widely used for paint, industrial production of alkyd resin, synthesis of high-grade lubricant, plasticizer, surfactant and raw materials of medicines, explosives and the like. Pentaerythritol is used primarily in the paint industry and can be used to make alkyd paints with improved hardness, gloss and durability of the paint film. It is also used as raw material of rosin ester for colour paint, varnish and printing ink, etc. and can be used for preparing drying oil, negative-fire coating and aviation lubricating oil, etc. Fatty acid esters of pentaerythritol are highly effective lubricants and plasticizers for polyvinyl chloride, and epoxy derivatives thereof are the starting materials for the production of nonionic surfactants. Pentaerythritol readily forms complexes with metals, is also used as a hard water softener in detergent formulations, and is also used in the production of pharmaceuticals, pesticides, and the like. Pentaerythritol contains four equivalent hydroxymethyl groups in the molecule and has high symmetry, so that the pentaerythritol is often used as a raw material for preparing multifunctional compounds. The pentaerythritol tetranitrate can be prepared by nitration of the mixture, and is a strong explosive; esterification to obtain pentaerythritol triacrylate for paint. 98-grade monopentaerythritol is mainly applied to high-performance flame retardants and can be matched with ammonium polyphosphate to obtain intumescent flame retardants.
Disclosure of Invention
The invention provides a method for producing 98-grade pentaerythritol with low energy consumption in order to overcome the defects in the prior art.
The invention is realized by the following technical scheme: the invention discloses a production method of 98-grade pentaerythritol with low energy consumption, which uses a set of novel production equipment, wherein the novel production equipment comprises a hydrolysis kettle for removing acetal through hydrolysis, a novel crystallization tank capable of cooling and crystallizing according to a program, a belt filter for solid-liquid separation, a fluidized bed for drying and a mechanical arm for packaging;
the production method of 98-grade pentaerythritol with low energy consumption specifically comprises the following steps:
(1) condensation reaction: adding formaldehyde, acetaldehyde and liquid alkali into a reaction kettle in a ratio of 4-16: 1: 1.1-1.3 in stages, reacting at the temperature of 35-65 ℃ for 1.5-2.5 hours, and keeping the temperature for 20-60 minutes;
(2) removing formaldehyde and adjusting pH: adding a certain amount of 27 mass percent hydrogen peroxide into the reaction kettle to oxidize excessive formaldehyde into formic acid until no residual formaldehyde is detected. Adding a certain amount of formic acid into the reaction kettle to adjust the pH value to be 4.5-5.5;
(3) hydrolysis: heating the neutralized condensation liquid in a hydrolysis kettle to 155-165 ℃ and keeping the condensation liquid under the pressure of 0.3-0.5 MPa for 1.8-2.1 hours, and exhausting gas;
(4) and (3) evaporation: after hydrolysis is finished, evaporating by using a normal-pressure continuous MVR evaporator, wherein the concentration of the evaporated final material is 1.10-1.20;
(5) and (3) crystallization: firstly, opening the steam of a novel crystallizing tank, boiling the materials to boil, closing the steam, opening the crystallizing tank to cool, adding 0.08kg/m when the temperature is reduced to 94-96 DEG C3～0.12kg/m3Seed crystals of 55 meshes to 65 meshes are maintained at the temperature of 92 ℃ to 98 ℃ for 1 to 2 hours, and are cooled to 70 ℃ to 85 ℃ for crystallization according to the speed of 4 ℃/h to 6 ℃/h;
(6) separation: carrying out solid-liquid separation on the crystallization liquid by using a belt filter;
(7) washing: spray washing the crystallized particles until the conductivity of the washing water is less than 0.18 ms/cm-0.22 ms/cm;
(8) and (3) drying and packaging: drying at 130-150 deg.c in fluidized bed, sieving, returning the sieved grain of less than 50 mesh to the crystallizing tank for re-dissolving and crystallizing, and bagging the sieved grain of more than 50 mesh according to the requirement of order.
In a preferred embodiment of the present invention, in the condensation reaction in step (1), formaldehyde, acetaldehyde and liquid alkali are added to a reaction kettle in stages at a ratio of 4 to 15: 1: 1.2, and the mixture is reacted at a temperature of 40 to 60 ℃ for 2 hours at a constant temperature for 30 minutes.
In a preferred embodiment of the present invention, in the process of adjusting PH in step (2), hydrogen peroxide is added to the reaction kettle to oxidize excess formaldehyde into formic acid, and simultaneously, a certain amount of formic acid is added to adjust PH so that PH becomes 5.
In the preferred embodiment of the present invention, in the hydrolysis process in step (3), the neutralized condensation liquid is fed into a hydrolysis kettle and heated to 160 ℃ and kept at a pressure of 0.4MPa for 2 hours, and simultaneously, the gas is discharged.
As a preferred embodiment of the invention, in the evaporation process in the step (4), an atmospheric continuous MVR evaporator is adopted for evaporation, and the concentration of the evaporated final material is 1.15.
As a preferred embodiment of the invention, in the crystallization process in the step (5), the steam of the novel crystallization tank is firstly opened, the material is boiled to be boiling, the steam is closed, the crystallization tank is opened to be cooled, the temperature is reduced to 95 ℃, and 0.1kg/m of steam is added360 mesh crystal seeds, maintaining the temperature of 95 ℃ for 1.5 hours, and cooling to 75-80 ℃ for crystallization at the speed of 5 ℃/h.
As a preferred embodiment of the present invention, in the washing process in the step (7), the crystalline particles are washed by spraying until the conductivity of the washing water is less than 0.2 ms/cm.
As a preferred embodiment of the present invention, in the drying and packaging process of step (8), the granules are dried at 140 ℃ by using a fluidized bed, and the granules are sieved.
The invention has the beneficial effects that: the invention discloses a low-energy-consumption 98-grade pentaerythritol production method, which adopts a sodium method to produce pentaerythritol intermittently, wherein the pentaerythritol is subjected to condensation reaction by taking formaldehyde and acetaldehyde as raw materials under the catalysis of liquid alkali, hydrogen peroxide is used for removing residual formaldehyde after the reaction is stopped, formic acid is used for adjusting the PH to about 5, and then the 98-grade pentaerythritol finished product is obtained through the working procedures of high-temperature high-pressure hydrolysis, efficient and continuous MVR evaporation, crystallization, separation, washing, drying, packaging and the like. The production method of the low-energy-consumption 98-grade pentaerythritol can realize the production of the low-energy-consumption 98-grade pentaerythritol and reduce the generation of byproducts, thereby improving the yield, ensuring that the removal rate of formaldehyde reaches 100 percent and removing the residual formaldehyde in the product. The method for producing 98-grade pentaerythritol with low energy consumption only uses a very small amount of steam in the evaporation process, thereby greatly reducing the investment of production cost. The low-energy-consumption 98-grade pentaerythritol production method can ensure the stability of material components in the 98-grade pentaerythritol clear liquid. The production method can improve the content of pentaerythritol in the solution, and the new profit is estimated to be increased by 400 ten thousand yuan/year by applying the production method.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Example 1: the invention discloses a production method of 98-grade pentaerythritol with low energy consumption, which specifically comprises the following steps: (1) condensation reaction: adding formaldehyde, acetaldehyde and liquid alkali into a reaction kettle in a ratio of 4: 1: 1.1 in stages, reacting for 1.5 hours at the temperature of 35 ℃, and keeping the temperature for 20 minutes; (2) removing formaldehyde and adjusting pH: adding a certain amount of 27 mass percent hydrogen peroxide into the reaction kettle to oxidize excessive formaldehyde into formic acid until no residual formaldehyde is detected. Adding a certain amount of formic acid into the reaction kettle to adjust the pH value to 4.5; (3) hydrolysis: heating the neutralized condensation liquid in a hydrolysis kettle to 155 ℃, keeping for 1.8 hours under the pressure condition of 0.3MPa, and exhausting; (4) and (3) evaporation: after the hydrolysis is finished, evaporating by adopting a normal-pressure continuous MVR evaporator, wherein the concentration of the evaporated final material is 1.10; (5) and (3) crystallization: opening the steam of the novel crystallizing tank, boiling the materials to boil, closing the steam, opening the crystallizing tank to cool, and adding 0.08kg/m when the temperature is reduced to 94 DEG C3Keeping the 55-mesh seed crystal at the temperature of 92 ℃ for 1 hour, and cooling to 70 ℃ for crystallization at the speed of 4 ℃/h; (6) separation: carrying out solid-liquid separation on the crystallization liquid by using a belt filter; (7) washing: washing the crystallized particles by adopting spray until the conductivity of washing water is less than 0.18 ms/cm; (8) and (3) drying and packaging: drying at 130 deg.C with fluidized bed, sieving, returning the sieved granules with particle size less than 50 meshes to crystallizing tank for re-dissolution and crystallization, and bagging the sieved granules with particle size greater than 50 meshes according to the order requirement.
Example 2: the production method of 98-grade pentaerythritol with low energy consumption specifically comprises the following stepsThe method comprises the following steps: (1) condensation reaction: adding formaldehyde, acetaldehyde and liquid alkali into a reaction kettle in a ratio of 4-15: 1: 1.2 in stages, reacting for 2 hours at the temperature of 40-60 ℃, and keeping the temperature for 30 minutes; (2) removing formaldehyde and adjusting pH: adding a certain amount of 27 mass percent hydrogen peroxide into the reaction kettle to oxidize excessive formaldehyde into formic acid until no residual formaldehyde is detected. Adding a certain amount of formic acid into the reaction kettle to adjust the pH value to 5; (3) hydrolysis: heating the neutralized condensation liquid in a hydrolysis kettle to 160 ℃, keeping for 2 hours under the pressure condition of 0.4MPa, and exhausting; (4) and (3) evaporation: after the hydrolysis is finished, evaporating by adopting a normal-pressure continuous MVR evaporator, wherein the concentration of the evaporated final material is 1.15; (5) and (3) crystallization: opening the steam of the novel crystallizing tank, boiling the material to boil, closing the steam, opening the crystallizing tank to cool, and adding 0.1kg/m when the temperature is reduced to 95 DEG C360-mesh seed crystal, maintaining the temperature of 95 ℃ for 1.5 hours, and cooling to 75-80 ℃ for crystallization at the speed of 5 ℃/h; (6) separation: carrying out solid-liquid separation on the crystallization liquid by using a belt filter; (7) washing: washing the crystallized particles by adopting spray until the conductivity of washing water is less than 0.2 ms/cm; (8) and (3) drying and packaging: drying at 130-150 deg.c in fluidized bed, sieving, returning the sieved grain of less than 50 mesh to the crystallizing tank for re-dissolving and crystallizing, and bagging the sieved grain of more than 50 mesh according to the requirement of order.
Example 3: the production method of 98-grade pentaerythritol with low energy consumption specifically comprises the following steps: (1) condensation reaction: adding formaldehyde, acetaldehyde and liquid caustic soda into a reaction kettle in a ratio of 16: 1: 1.3 in stages, reacting for 2.5 hours at the temperature of 65 ℃, and keeping the temperature for 60 minutes; (2) removing formaldehyde and adjusting pH: adding a certain amount of 27 mass percent hydrogen peroxide into the reaction kettle to oxidize excessive formaldehyde into formic acid until no residual formaldehyde is detected. Adding a certain amount of formic acid into the reaction kettle to adjust the pH value to be 5.5; (3) hydrolysis: heating the neutralized condensation liquid in a hydrolysis kettle to 165 ℃, keeping for 2.1 hours under the pressure condition of 0.5MPa, and exhausting; (4) and (3) evaporation: after the hydrolysis is finished, evaporating by adopting a normal-pressure continuous MVR evaporator, wherein the concentration of the evaporated final material is 1.20; (5) and (3) crystallization: the steam of the novel crystallizing tank is firstly started,boiling the materials to boil, closing steam, opening crystallization tank, cooling, adding 0.12kg/m when cooling to 96 deg.C3Keeping the 65-mesh seed crystal at 98 ℃ for 2 hours, and cooling to 85 ℃ according to the speed of 6 ℃/h for crystallization; (6) separation: carrying out solid-liquid separation on the crystallization liquid by using a belt filter; (7) washing: washing the crystallized particles by adopting spray until the conductivity of washing water is less than 0.22 ms/cm; (8) and (3) drying and packaging: drying at 140 ℃ by adopting a fluidized bed, sieving the particles, returning the particles with the particle size of less than 50 meshes to a crystallizing tank for re-dissolution and crystallization, and bagging the particles with the particle size of more than 50 meshes according to the requirement of an order after sieving.
In the three embodiments, the yield of the embodiment 1 and the yield of the embodiment 3 are better than that of the prior art through comparison, wherein the production effect of the embodiment 2 is the best, and through practical application, the production method provided by the invention can enable chemical industry enterprises to increase the profit by 400 ten thousand yuan per year.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. A production method of 98-grade pentaerythritol with low energy consumption is characterized in that: the production method of the low-energy-consumption 98-grade pentaerythritol specifically comprises the following steps:
(1) condensation reaction:
adding formaldehyde, acetaldehyde and liquid alkali into a reaction kettle in a ratio of 4-16: 1: 1.1-1.3 in stages, reacting at the temperature of 35-65 ℃ for 1.5-2.5 hours, and keeping the temperature for 20-60 minutes;
(2) removing formaldehyde and adjusting pH:
adding a certain amount of 27 mass percent hydrogen peroxide into the reaction kettle to oxidize excessive formaldehyde into formic acid until no residual formaldehyde is detected; adding a certain amount of formic acid into the reaction kettle to adjust the pH value to be 4.5-5.5;
(3) hydrolysis:
heating the neutralized condensation liquid in a hydrolysis kettle to 155-165 ℃ and keeping the condensation liquid under the pressure of 0.3-0.5 MPa for 1.8-2.1 hours, and exhausting gas;
(4) and (3) evaporation:
after hydrolysis is finished, evaporating by using a normal-pressure continuous MVR evaporator, wherein the concentration of the evaporated final material is 1.10-1.20;
(5) and (3) crystallization:
firstly, opening the steam of a novel crystallizing tank, boiling the materials to boil, closing the steam, opening the crystallizing tank to cool, adding 0.08kg/m when the temperature is reduced to 94-96 DEG C3～0.12kg/m3Seed crystals of 55 meshes to 65 meshes are maintained at the temperature of 92 ℃ to 98 ℃ for 1 to 2 hours, and are cooled to 70 ℃ to 85 ℃ for crystallization according to the speed of 4 ℃/h to 6 ℃/h;
(6) separation:
carrying out solid-liquid separation on the crystallization liquid by using a belt filter;
(7) washing:
spray washing the crystallized particles until the conductivity of the washing water is less than 0.18 ms/cm-0.22 ms/cm;
(8) and (3) drying and packaging:
drying at 130-150 deg.c in fluidized bed, sieving, returning the sieved grain of less than 50 mesh to the crystallizing tank for re-dissolving and crystallizing, and bagging the sieved grain of more than 50 mesh according to the requirement of order.
2. The method for producing pentaerythritol with low energy consumption and 98 grades according to claim 1, is characterized in that: in the condensation reaction in the step (1), formaldehyde, acetaldehyde and liquid alkali in a ratio of 4-15: 1: 1.2 are added into a reaction kettle in stages.
3. The method for producing pentaerythritol with low energy consumption grade 98 as claimed in claim 1 or 2, characterized in that: in the condensation reaction in the step (1), the reaction is carried out for 2 hours at the temperature of 40-60 ℃, and the temperature is kept for 30 minutes.
4. The method for producing pentaerythritol with low energy consumption grade 98 as claimed in claim 1 or 2, characterized in that: and (3) in the process of removing formaldehyde and adjusting pH in the step (2), adding hydrogen peroxide into the reaction kettle to oxidize excessive formaldehyde into formic acid, and simultaneously adding a certain amount of formic acid to adjust pH to 5.
5. The method for producing pentaerythritol with low energy consumption grade 98 as claimed in claim 1 or 2, characterized in that: and (3) in the hydrolysis process of the step (3), the neutralized condensation liquid enters a hydrolysis kettle, is heated to 160 ℃, stays for 2 hours under the pressure condition of 0.4MPa, and is exhausted.
6. The method for producing pentaerythritol with low energy consumption grade 98 as claimed in claim 1 or 2, characterized in that: and (4) in the evaporation process of the step (4), evaporating by adopting a normal-pressure continuous MVR evaporator, wherein the concentration of the evaporated final material is 1.15.
7. The method for producing pentaerythritol with low energy consumption grade 98 as claimed in claim 1 or 2, characterized in that: in the crystallization process in the step (5), firstly, the steam of the novel crystallization tank is opened, the material is boiled to be boiling, the steam is closed, the crystallization tank is opened to cool, the temperature is reduced to 95 ℃, and 0.1kg/m of steam is added360 mesh crystal seeds, maintaining the temperature of 95 ℃ for 1.5 hours, and cooling to 75-80 ℃ for crystallization at the speed of 5 ℃/h.
8. The method for producing pentaerythritol with low energy consumption grade 98 as claimed in claim 1 or 2, characterized in that: and (4) in the washing process of the step (7), spray washing is adopted to wash the crystallized particles until the conductivity of the washing water is less than 0.2 ms/cm.
9. The method for producing pentaerythritol with low energy consumption grade 98 as claimed in claim 1 or 2, characterized in that: in the drying and packaging process in the step (8), drying is carried out at 140 ℃ by adopting a fluidized bed, and the particles are sieved.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111683565.0A CN114315517A (en) | 2021-12-31 | 2021-12-31 | Production method of low-energy-consumption 98-grade pentaerythritol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202111683565.0A CN114315517A (en) | 2021-12-31 | 2021-12-31 | Production method of low-energy-consumption 98-grade pentaerythritol |
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| CN115806473A (en) * | 2022-12-08 | 2023-03-17 | 赤峰瑞阳化工有限公司 | Method for removing pentaerythritol formal macromolecular impurities |
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