CN114085127A - Crystallization separation method of pentaerythritol - Google Patents
Crystallization separation method of pentaerythritol Download PDFInfo
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- CN114085127A CN114085127A CN202111458094.3A CN202111458094A CN114085127A CN 114085127 A CN114085127 A CN 114085127A CN 202111458094 A CN202111458094 A CN 202111458094A CN 114085127 A CN114085127 A CN 114085127A
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 86
- 230000008025 crystallization Effects 0.000 title claims abstract description 86
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000000926 separation method Methods 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 46
- 239000013078 crystal Substances 0.000 claims abstract description 44
- 239000002245 particle Substances 0.000 claims abstract description 41
- 238000005406 washing Methods 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 238000001816 cooling Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 7
- 238000004806 packaging method and process Methods 0.000 claims description 6
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 125000003158 alcohol group Chemical group 0.000 claims description 2
- 235000013399 edible fruits Nutrition 0.000 claims 2
- 239000010409 thin film Substances 0.000 claims 2
- 238000012858 packaging process Methods 0.000 claims 1
- 230000000630 rising effect Effects 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000011068 loading method Methods 0.000 abstract 1
- 238000000197 pyrolysis Methods 0.000 abstract 1
- 239000007921 spray Substances 0.000 abstract 1
- 229940059574 pentaerithrityl Drugs 0.000 description 27
- 239000003973 paint Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin 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
- 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
- 239000004698 Polyethylene 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
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229960004321 pentaerithrityl tetranitrate Drugs 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 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
Classifications
-
- 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
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D33/00—Filters with filtering elements which move during the filtering operation
- B01D33/04—Filters with filtering elements which move during the filtering operation with filtering bands or the like supported on cylinders which are impervious for filtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0036—Crystallisation on to a bed of product crystals; Seeding
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a crystallization separation method of pentaerythritol, which comprises the steps of firstly adding 90-alcohol solution into a crystallization tank, cooling to 95 ℃ in the first stage, wherein the cooling speed is 5 ℃/h; in the second stage, the temperature is reduced to 90 ℃, the temperature reduction speed is 2 ℃/h, and 60-mesh 1% pentaerythritol particles are added as seed crystals; in the third stage, the constant temperature is kept at 90 ℃ for 2 hours; the temperature is reduced to 70 ℃ in the fourth stage, and the temperature reduction speed is 5 ℃/h; then adding 0.5m of washing water for carrying out the dry distillation, heating to 80 ℃, eliminating the saturation, carrying out solid-liquid separation on the crystallization liquid by using a belt filter, washing with primary water at 25 ℃, and carrying out spray washing on the crystallization particles; drying at 140 deg.C with fluidized bed, feeding into finished product tank, and loading according to the order. The invention adopts a three-stage crystallization process, and the prepared pentaerythritol crystals have good fluidity, good dispersibility, large crystals, full particles, easy filtration, simple operation and less equipment investment.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a crystallization separation method of pentaerythritol.
Background
Pentaerythritol is an organic intermediate with wide application, can be used for manufacturing high-grade temperature-resistant lubricating grease, high-grade resin, transparent photopolymerization synthetic material and flame-retardant material, is an excellent non-toxic additive for polyethylene and polyvinyl chloride, and has good ductility and ageing resistance. Is also commonly used in the paint industry as a raw material for alkyd paints, and can improve the hardness, gloss and durability of paint films; it is also used as a raw material for rosin esters such as printing inks for varnishes and paints, and can produce flame-retardant coatings, drying oils, aviation oils, and the like. Pentaerythritol tetranitrate is an explosive made from pentaerythritol. Pentaerythritol fatty acid esters are used as plasticizers and stabilizers for polyvinyl chloride resins, and pentaerythritol is used in the production of pharmaceuticals, agricultural chemicals, lubricating oils, and the like. Pentaerythritol is prepared by condensation of formaldehyde and acetaldehyde as raw materials in the presence of an alkaline catalyst, and pentaerythritol is usually produced by a traditional crystallization process in the prior art, but pentaerythritol particles produced by the traditional crystallization process in the prior art are basically pseudo particles, the particle size distribution of the pentaerythritol particles is not uniform, fine powder is more, the product appearance is poor, and the fine powder has the possibility of dust explosion in the using process.
Disclosure of Invention
The invention provides a crystallization separation method of pentaerythritol in order to overcome the defects in the prior art.
The invention is realized by the following technical scheme: the invention discloses a crystallization separation method of pentaerythritol, which uses a set of novel crystallization and separation equipment, wherein the novel crystallization and separation equipment comprises a novel crystallization tank capable of crystallizing according to a crystallization procedure, a belt filter for solid-liquid separation, a fluidized bed for drying and a finished product tank for containing a finished product; the crystallization separation method of pentaerythritol comprises 8 steps of cooling, crystallization, crystal growing, crystallization, heating, centrifugation, washing, drying and packaging in sequence;
the crystallization separation method of pentaerythritol specifically comprises the following steps:
(1) cooling: adding the 90-degree quaternary alcohol solution into a novel crystallization tank, cooling to 90-100 ℃ in the first stage, wherein the cooling speed is 4-6 ℃/h, and the stirring speed is adjusted to 75-85 r/min;
(2) and (3) crystallization: a second stage crystallization process, wherein the temperature is reduced to 85-95 ℃ in the second stage, the temperature reduction speed is 1-3 ℃/h, and pentaerythritol particles with the mass percentage of 0.8-1.2 percent of 55-65 meshes are added as seed crystals;
(3) growing the grains: in the third stage of crystal growing, the temperature in the novel crystallizing tank is kept constant at 85-95 ℃ for 1-2 hours;
(4) and (3) crystallization: the fourth stage is a crystallization process, the temperature of the fourth stage is reduced to 65-75 ℃ in a novel crystallization tank, and the temperature reduction speed is 4-6 ℃/h;
(5) and (3) heating: the fourth stage is a temperature rise process, washing water with the volume of 0.4-0.6 m for carrying out thin-wall dry-mass dry-mass dry;
(6) centrifuging: and carrying out solid-liquid separation on the crystal liquid subjected to the temperature rise process by using a belt filter, wherein the speed of a filter belt of the belt filter is 1-3 m/min.
(7) Washing: washing the crystal particles after solid-liquid separation with primary water at the temperature of 20-30 ℃, and washing the crystal particles in a spraying manner;
(8) and (3) drying and packaging: drying the washed crystal particles at 135-145 ℃ by a fluidized bed, feeding the dried crystal particles into a finished product tank, and bagging the dried crystal particles according to the specification according to the requirement of an order.
As a preferred embodiment of the invention, in the cooling process in the step (1), the temperature is reduced to 95 ℃ in the first stage, the cooling speed is 5 ℃/h, and the stirring speed is adjusted to 80 r/min.
As a preferred embodiment of the invention, in the crystallization process in the step (2), the temperature is reduced to 90 ℃ in the second stage, the temperature reduction speed is 2 ℃/h, and 60-mesh pentaerythritol particles with the mass percent of 1% are added as seed crystals.
In the preferred embodiment of the invention, in the crystal growing process in the step (3), the third stage is to keep the constant temperature of 90 ℃ in the novel crystallizing tank for 1.5 hours.
In the crystallization process in the step (4), the temperature is reduced to 70 ℃ in the novel crystallization tank at the fourth stage, wherein the temperature reduction speed is 5 ℃/h.
In a preferred embodiment of the invention, in the step (5), during the temperature rise, washing water with the volume of 0.5m is added, and the temperature is raised to 80 ℃ in the novel crystallizing tank to eliminate the saturation of the crystallization liquid.
As a preferred embodiment of the present invention, the belt speed of the belt filter during the centrifugation in the step (6) is 1.5 m/min.
In a preferred embodiment of the present invention, in the washing step (7), the crystallized particles after the solid-liquid separation are washed with primary water having a water temperature of 25 ℃.
As a preferred embodiment of the present invention, in the step (8) of drying and packaging, the washed crystalline particles are dried at a temperature of 140 ℃ by using a fluidized bed
The invention has the beneficial effects that: the invention improves and researches pentaerythritol particles and develops a novel pentaerythritol crystallization and separation technology. The invention adopts a three-stage crystallization process, and the prepared pentaerythritol crystals have good fluidity, good dispersibility, large crystals, full particles and easy filtration. The crystallization separation method of pentaerythritol is simple to operate, has low equipment investment and is worthy of wide popularization and application.
Detailed Description
The present invention will be described in detail with reference to specific embodiments.
Example 1: the invention discloses a crystallization separation method of pentaerythritol, which uses a set of novel crystallization and separation equipment, wherein the equipment comprises a novel crystallization tank capable of crystallizing according to a crystallization procedure, a belt filter for solid-liquid separation, a fluidized bed for drying and a finished product tank for containing a finished product; the crystallization separation method of pentaerythritol comprises 8 steps of cooling, crystallization, crystal growing, crystallization, heating, centrifugation, washing, drying and packaging in sequence; firstly, adding 90-season alcohol solution into a crystallization tank, cooling to 95 ℃ in the first stage, wherein the cooling speed is 5 ℃/h, and the stirring speed is adjusted to 80 r/min; in the second stage, the temperature is reduced to 90 ℃, the temperature reduction speed is 2 ℃/h, and 60-mesh 1% pentaerythritol particles are added as seed crystals; in the third stage, the constant temperature is kept at 90 ℃ for 1-2 hours; the temperature is reduced to 70 ℃ in the fourth stage, and the temperature reduction speed is 5 ℃/h; then adding 0.5m of washing water for the cultivation under high temperature to 80 ℃, eliminating saturation, carrying out solid-liquid separation on the crystallization liquid by using a belt filter, wherein the belt speed of the belt filter is 1.5 m/min, washing with 25 ℃ primary water, and spraying and washing the crystallization particles; and finally, drying by adopting a fluidized bed at the temperature of 140 ℃, then feeding into a finished product tank, and bagging according to the specification according to the order requirement.
Example 2: the crystallization separation method of pentaerythritol specifically comprises the following steps: adding the 90-season alcohol solution into a novel crystallization tank, cooling to 90 ℃ in the first stage, wherein the cooling speed is 4 ℃/h, and the stirring speed is adjusted to 75 r/min; a second stage crystallization process, wherein the temperature is reduced to 85 ℃ in the second stage, the temperature reduction speed is 1 ℃/h, and pentaerythritol particles with the mass percent of 0.8 percent of 55 meshes are added as seed crystals; in the third stage of crystal growing process, the third stage of crystal growing process is to keep the constant temperature of 85 ℃ in the novel crystallizing tank for 1 hour; the fourth stage is a crystallization process, the temperature of the fourth stage is reduced to 65 ℃ in a novel crystallization tank, and the temperature reduction speed is 4 ℃/h; the fourth stage is a temperature rise process, washing water with the volume of 0.4m is added during temperature rise, the temperature is raised to 75 ℃ in a novel crystallizing tank, and the saturation of the crystallization liquid is eliminated; carrying out solid-liquid separation on the crystal liquid subjected to the temperature rise process by using a belt filter, wherein the belt speed of the belt filter is 1.2 m/min; washing the crystallized particles after solid-liquid separation with primary water with the water temperature of 20 ℃, and washing the crystallized particles in a spraying manner; drying the washed crystal particles at 135 ℃ by adopting a fluidized bed, feeding the dried crystal particles into a finished product tank, and bagging the dried crystal particles according to the specification according to the requirement of an order.
Example 3: the crystallization separation method of pentaerythritol specifically comprises the following steps: adding 90-degree alcohol solution into a novel crystallization tank, cooling to 100 ℃ in the first stage, wherein the cooling speed is 6 ℃/h, and the stirring speed is adjusted to 85 r/min; a second stage crystallization process, wherein the temperature is reduced to 95 ℃ in the second stage, the temperature reduction speed is 3 ℃/h, and pentaerythritol particles with the mass percent of 1.2 percent of 65 meshes are added as seed crystals; in the third stage of crystal growing process, the third stage is to keep the constant temperature of 95 ℃ in the novel crystallizing tank for 2 hours; the fourth stage is a crystallization process, the temperature of the fourth stage is reduced to 75 ℃ in a novel crystallization tank, and the temperature reduction speed is 6 ℃/h; the fourth stage is a temperature rise process, washing water with the volume of 0.6m is added during temperature rise, the temperature is raised to 85 ℃ in a novel crystallizing tank, and the saturation of the crystallization liquid is eliminated; carrying out solid-liquid separation on the crystal liquid subjected to the temperature rise process by using a belt filter, wherein the speed of a filter belt of the belt filter is 1.7 m/min; washing the crystal particles after solid-liquid separation with primary water with the water temperature of 30 ℃, and washing the crystal particles in a spraying manner; drying the washed crystal particles at 145 ℃ by adopting a fluidized bed, feeding the dried crystal particles into a finished product tank, and bagging the dried crystal particles according to the specification according to the requirement of an order.
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 (10)
1. A crystallization separation method of pentaerythritol is characterized in that: the crystallization and separation method of pentaerythritol uses a set of novel crystallization and separation equipment, wherein the novel crystallization and separation equipment comprises a novel crystallization tank capable of crystallizing according to a crystallization procedure, a belt filter for solid-liquid separation, a fluidized bed for drying and a finished product tank for containing finished products; the crystallization separation method of pentaerythritol comprises 8 steps of cooling, crystallization, crystal growing, crystallization, heating, centrifugation, washing, drying and packaging in sequence;
the crystallization separation method of pentaerythritol specifically comprises the following steps:
(1) cooling:
adding the 90-degree quaternary alcohol solution into a novel crystallization tank, cooling to 90-100 ℃ in the first stage, wherein the cooling speed is 4-6 ℃/h, and the stirring speed is adjusted to 75-85 r/min;
(2) and (3) crystallization:
a second stage crystallization process, wherein the temperature is reduced to 85-95 ℃ in the second stage, the temperature reduction speed is 1-3 ℃/h, and pentaerythritol particles with the mass percentage of 0.8-1.2 percent of 55-65 meshes are added as seed crystals;
(3) growing the grains:
in the third stage of crystal growing, the temperature in the novel crystallizing tank is kept constant at 85-95 ℃ for 1-2 hours;
(4) and (3) crystallization:
the fourth stage is a crystallization process, the temperature of the fourth stage is reduced to 65-75 ℃ in a novel crystallization tank, and the temperature reduction speed is 4-6 ℃/h;
(5) and (3) heating:
the fourth stage is a temperature rise process, washing water with the volume of 0.4-0.6 m for carrying out thin-wall dry-mass dry-mass dry;
(6) centrifuging:
carrying out solid-liquid separation on the crystallization liquid subjected to the temperature rise process by using a belt filter, wherein the speed of a filter belt of the belt filter is 1-3 m/min;
(7) washing:
washing the crystal particles after solid-liquid separation with primary water at the temperature of 20-30 ℃, and washing the crystal particles in a spraying manner;
(8) and (3) drying and packaging:
drying the washed crystal particles at 135-145 ℃ by a fluidized bed, feeding the dried crystal particles into a finished product tank, and bagging the dried crystal particles according to the specification according to the requirement of an order.
2. The method for separating pentaerythritol through crystallization according to claim 1, wherein: in the cooling process of the step (1), the temperature is reduced to 95 ℃ in the first stage, the cooling speed is 5 ℃/h, and the stirring speed is adjusted to 80 r/min.
3. The method for separating pentaerythritol by crystallization according to claim 1 or 2, characterized in that: in the crystallization process of the step (2), the temperature is reduced to 90 ℃ in the second stage, and the temperature reduction speed is 2 ℃/h.
4. The method for separating pentaerythritol by crystallization according to claim 1 or 2, characterized in that: and (3) in the crystallization process in the step (2), adding 1% of pentaerythritol particles with the mass percentage of 60 meshes as seed crystals.
5. The method for separating pentaerythritol by crystallization according to claim 1 or 2, characterized in that: in the crystal growing process in the step (3), the third stage is to keep the constant temperature of 90 ℃ in the novel crystallizing tank for 1.5 hours.
6. The method for separating pentaerythritol by crystallization according to claim 1 or 2, characterized in that: in the crystallization process in the step (4), the temperature is reduced to 70 ℃ in the novel crystallization tank in the fourth stage, and the temperature reduction speed is 5 ℃/h.
7. The method for separating pentaerythritol by crystallization according to claim 1 or 2, characterized in that: and (5) in the temperature rising process of the step (5), adding washing water with the volume of 0.5m for carrying out thin film fruit bearing and carrying out thin film fruit bearing, and raising the temperature to 80 ℃ in a novel crystallizing tank to eliminate the saturation of the crystallization liquid.
8. The method for separating pentaerythritol by crystallization according to claim 1 or 2, characterized in that: and (3) in the centrifugation process of the step (6), the filter belt speed of the belt filter is 1.5 m/min.
9. The method for separating pentaerythritol by crystallization according to claim 1 or 2, characterized in that: in the washing process of the step (7), the crystallized particles after solid-liquid separation are washed with primary water with the water temperature of 25 ℃.
10. The method for separating pentaerythritol by crystallization according to claim 1 or 2, characterized in that: and (3) in the drying and packaging process in the step (8), drying the washed crystal particles at 140 ℃ by adopting a fluidized bed.
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| CN202111458094.3A CN114085127A (en) | 2021-12-02 | 2021-12-02 | Crystallization separation method of pentaerythritol |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696158A (en) * | 2009-09-30 | 2010-04-21 | 濮阳市鹏鑫化工有限公司 | Method for preparing pentaerythritol and dipentaerythritol |
| CN104447202A (en) * | 2014-11-14 | 2015-03-25 | 江苏开磷瑞阳化工股份有限公司 | Production method of pentaerythritol by virtue of potassium method |
| CN105693467A (en) * | 2016-04-06 | 2016-06-22 | 内蒙古宜化化工有限公司 | Energy-saving production method of pentaerythritol |
| CN109438182A (en) * | 2018-12-14 | 2019-03-08 | 赤峰瑞阳化工有限公司 | A kind of production system and its production technology of 99 grades of pentaerythrites |
-
2021
- 2021-12-02 CN CN202111458094.3A patent/CN114085127A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101696158A (en) * | 2009-09-30 | 2010-04-21 | 濮阳市鹏鑫化工有限公司 | Method for preparing pentaerythritol and dipentaerythritol |
| CN104447202A (en) * | 2014-11-14 | 2015-03-25 | 江苏开磷瑞阳化工股份有限公司 | Production method of pentaerythritol by virtue of potassium method |
| CN105693467A (en) * | 2016-04-06 | 2016-06-22 | 内蒙古宜化化工有限公司 | Energy-saving production method of pentaerythritol |
| CN109438182A (en) * | 2018-12-14 | 2019-03-08 | 赤峰瑞阳化工有限公司 | A kind of production system and its production technology of 99 grades of pentaerythrites |
Non-Patent Citations (1)
| Title |
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| 陈珍: "L-丙交酯结晶过程的研究", 中国优秀硕士学位论文全文数据库工程科技Ⅰ辑 * |
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