CN117504345A - Novel maltol pipeline crystallization process - Google Patents
Novel maltol pipeline crystallization process Download PDFInfo
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- CN117504345A CN117504345A CN202311396158.0A CN202311396158A CN117504345A CN 117504345 A CN117504345 A CN 117504345A CN 202311396158 A CN202311396158 A CN 202311396158A CN 117504345 A CN117504345 A CN 117504345A
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- 238000002425 crystallisation Methods 0.000 title claims abstract description 75
- 230000008025 crystallization Effects 0.000 title claims abstract description 70
- XPCTZQVDEJYUGT-UHFFFAOYSA-N 3-hydroxy-2-methyl-4-pyrone Chemical compound CC=1OC=CC(=O)C=1O XPCTZQVDEJYUGT-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 30
- HYMLWHLQFGRFIY-UHFFFAOYSA-N Maltol Natural products CC1OC=CC(=O)C1=O HYMLWHLQFGRFIY-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 229940043353 maltol Drugs 0.000 title claims abstract description 28
- 238000001816 cooling Methods 0.000 claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 54
- 239000012267 brine Substances 0.000 claims description 48
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 48
- 239000007788 liquid Substances 0.000 claims description 29
- 238000007599 discharging Methods 0.000 claims description 20
- 238000000926 separation method Methods 0.000 claims description 18
- 239000000243 solution Substances 0.000 claims description 16
- 238000009835 boiling Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 239000013078 crystal Substances 0.000 claims description 13
- 238000005086 pumping Methods 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- 238000004064 recycling Methods 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 9
- 238000000859 sublimation Methods 0.000 claims description 9
- 230000008022 sublimation Effects 0.000 claims description 9
- 239000000463 material Substances 0.000 abstract description 20
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000000428 dust Substances 0.000 abstract description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 5
- 238000007710 freezing Methods 0.000 description 5
- 230000008014 freezing Effects 0.000 description 5
- YIKYNHJUKRTCJL-UHFFFAOYSA-N Ethyl maltol Chemical compound CCC=1OC=CC(=O)C=1O YIKYNHJUKRTCJL-UHFFFAOYSA-N 0.000 description 4
- 229940093503 ethyl maltol Drugs 0.000 description 4
- 239000000796 flavoring agent Substances 0.000 description 4
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000004821 distillation Methods 0.000 description 3
- 235000013355 food flavoring agent Nutrition 0.000 description 3
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 3
- 239000000413 hydrolysate Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 235000013361 beverage Nutrition 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000011265 semifinished product Substances 0.000 description 2
- 229910000619 316 stainless steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000006798 ring closing metathesis reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000006257 total synthesis reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 235000014101 wine Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
- C07D309/34—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D309/36—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with oxygen atoms directly attached to ring carbon atoms
- C07D309/40—Oxygen atoms attached in positions 3 and 4, e.g. maltol
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/02—Crystallisation from solutions
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Saccharide Compounds (AREA)
Abstract
The utility model provides a novel process for crystallizing a maltol pipeline, and belongs to the technical field of maltol production. According to the utility model, a specific pipeline crystallization reactor is utilized to replace a traditional two-step method kettle for cooling crystallization, rapid cooling crystallization of materials in a pipeline is realized through pipe diameter change of the pipeline crystallization reactor and material flow rate control, the section yield is improved, the production efficiency is improved, the influence of dust generation is reduced, and the environment-friendly benefit is realized.
Description
Technical Field
The utility model belongs to the technical field of maltol production, and particularly relates to a novel process for crystallizing a maltol pipeline.
Background
The maltol has the special flavor of the burnt cream hard candy, and is a good flavoring agent and a low-intensity sweetener for food and beverage; can be widely used as flavoring agent for flavoring essence, flavoring agent for flavoring and sweet taste of food, beverage, and wine. In recent years, the application field of maltol is expanding, the dosage is increasing, and the export quantity is rising.
The maltol synthesis process is various, such as Qu Suanfa (semisynthesis), jiao Meikang acid process, furfuryl alcohol process, furfural process (total synthesis), electrolytic oxidation process, organic ring closure process, etc. The furfural method is a method commonly used in the industry at present, and the production process is divided into a Grignard working section, a chlorination working section, a sublimation working section, a crystallization working section and a drying working section. In the production of maltol/maltol, the semi-finished product is added with ethanol for boiling in a crystallization section, impurities are removed, then the semi-finished product is placed into a freezing kettle for crystallization, the materials are placed into a centrifuge for spin-drying after crystallization, and the centrifuged wet finished product is sent for drying. At present, crystallization is mostly carried out in a kettle cooling mode in industry.
According to the utility model, after a proper amount of ethanol is needed to be added into the ethyl maltol crude product to crystallize in the crystallization kettle, the ethyl maltol is centrifuged by a centrifuge, the obtained solid is ethyl maltol, the obtained liquid is ethyl maltol-containing ethanol mother liquor, the ethanol mother liquor is distilled to recover ethanol, and the ethanol obtained after distillation can be further added into the crystallizer for crystallization and repeated use.
Also, as disclosed in patent CN108299362B, a method for separating impurities from crude maltol comprises: a. filtering the hydrolyzed material and cooling to 30-35 ℃; b. pumping the hydrolysate into an extraction mixer, and pumping chloroform at the same time to fully mix the hydrolysate and the chloroform; c. feeding the mixed solution into a layering device, feeding the layered light phase into a hydrolysate collecting tank, feeding the lower heavy phase into a chloroform collecting tank, putting the chloroform collecting tank into a distillation kettle for distillation to recover chloroform, and feeding the distilled material into a sublimation kettle for sublimation; d. pumping the light phase material in the hydrolysis collecting tank into a neutralization kettle, regulating the PH to 2.5-3.5, reducing the temperature to 40-45 ℃, putting the material into a crystallizer for freezing crystallization, and delivering the material into a sublimation kettle for sublimation after centrifugal drying.
The cooling crystallization mode of the kettle has the advantages that the reaction time of the severe chlorination reaction in the kettle is long, more byproducts are generated, the product conversion rate is low, the labor cost is increased, the operation stability is poor, and the labor intensity is high.
Disclosure of Invention
The utility model aims to provide a novel maltol pipeline crystallization process aiming at the problems of low conversion rate, more byproducts and low production efficiency of the existing kettle type cooling.
In order to achieve the above purpose, the technical scheme adopted by the utility model is as follows:
a pipeline crystallization reactor comprises a 4-section pipeline and a filter,
a feed inlet is formed in the top of a first section of pipeline in the 4 sections of pipelines, a fourth section of pipeline is connected with a filter, and a discharge outlet is formed in the bottom of the filter;
an inclined pipeline is arranged at the position, close to the discharge hole, of the filter to discharge filtrate;
the outside of the 4 sections of pipelines is provided with a jacket, a brine outlet is arranged at the position of the jacket close to the feed inlet, and a brine inlet is arranged at the position of the jacket close to the filter.
Further, the pipe diameter of the 4-section pipeline is as follows: the diameter of the first section of pipeline is 48-52mm, preferably 50mm; the diameter of the second section of pipeline is 62-65mm, preferably 65mm; the diameter of the third section of pipeline is 78-82mm, preferably 80mm; the diameter of the fourth section of pipeline is 95-100mm, preferably 100mm.
Preferably, the pipe diameter of the 4-section pipe is as follows: the diameter of the first section of pipeline is 50mm, the diameter of the second section of pipeline is 65mm, the diameter of the third section of pipeline is 80mm, and the diameter of the fourth section of pipeline is 100mm.
Further, the separator is a horizontal centrifugal separator, and is made of 316 stainless steel.
The application of the pipeline crystallization reactor in the production of maltol.
A method of maltol pipeline crystallization comprising the steps of:
(1) Introducing frozen brine into a jacket of the pipeline crystallization reactor through a brine inlet, then pumping ethanol solution obtained after high-temperature boiling into the pipeline crystallization reactor through a feed inlet, cooling through a 4-section pipeline, and performing solid-liquid separation through a filter;
(2) And discharging the solid crystals obtained by solid-liquid separation from a discharge hole, drying, discharging the liquid from an inclined pipeline, and purifying and recycling.
Further, the temperature of the frozen brine is-15 to-25 ℃. Preferably, the temperature of the frozen brine is-20 ℃.
Further, the flow rate of the frozen brine is 5-8m 3 Preferably 6m 3 /h。
Further, the ethanol solution after high-temperature boiling is a product obtained by adding ethanol into a product obtained in a sublimation working section in the production process of maltol and after high-temperature boiling.
Further, the feeding flow rate of the ethanol solution is 0.4-1m 3 Preferably the feed flow rate is 0.8m 3 /h。
Compared with the prior art, the utility model has the following beneficial effects:
1. the maltol pipeline crystallization method breaks through the traditional cooling mode, can realize instant cooling, improves the production efficiency, reduces the generation of dust, and has environmental protection benefits.
2. The pipe crystallization reactor is provided with the jacket brine to realize physical cooling, the retention time of the materials in the pipe diameter is adjusted by controlling the flow rate and the pipe diameter of the materials, the full and rapid cooling is achieved, the continuity is strong, the operation stability is greatly improved, the yield of the working section is improved by 5%, the pipe crystallization reactor has larger economic benefit, and finally the obtained crystal particles are better.
3. The kettle type cooling is rough, the maintenance and replacement are troublesome, the manual control is tedious, the error is large, the cooling volume of the pipeline crystallization reactor is small, and the production is convenient through flow control.
Drawings
FIG. 1 is a schematic structural view of a pipe crystallization reactor according to the present utility model;
wherein, 1-first section pipeline, 2-second section pipeline, 3-third section pipeline, 4-fourth section pipeline, 5-jacket, 6-filter, 7-feed inlet, 8-discharge gate.
Detailed Description
The following non-limiting examples will enable those of ordinary skill in the art to more fully understand the utility model and are not intended to limit the utility model in any way. The following is merely exemplary of the scope of the utility model as claimed and many variations and modifications of the utility model will be apparent to those skilled in the art in light of the disclosure, which are intended to be within the scope of the utility model as claimed.
The utility model is further illustrated by means of the following specific examples. The various chemical reagents used in the examples of the present utility model were obtained by conventional commercial means unless otherwise specified. Wherein the ethanol solution after high-temperature boiling is a product obtained by adding ethanol into a product obtained by a sublimation working section in the production process of maltol, and 1200L of ethanol solution is added into each 400kg of the product obtained by the sublimation working section.
Example 1
A maltol pipeline crystallization process comprising the steps of:
(1) Referring to fig. 1, a pipe crystallization reactor is provided, which is divided into 4 sections of pipes and a filter (6);
the top of a first section of pipeline (1) in the 4 sections of pipelines is provided with a feed inlet, a fourth section of pipeline (4) is connected with a filter (6), and the bottom of the filter (6) is provided with a discharge outlet (8);
an inclined pipeline is arranged at the position, close to the discharge hole (7), of the filter (6) to discharge filtrate; a jacket (5) is arranged outside the 4-section pipeline, a brine outlet is arranged at the position, close to the feed inlet (7), of the jacket (5), a brine inlet is arranged at the position, close to the filter (6), of the jacket (5), and the brine temperature is-20 ℃;
the pipe diameter of the 4-section pipeline is as follows: the diameter of the first section of pipeline (1) is 50mm, the diameter of the second section of pipeline (2) is 65mm, the diameter of the third section of pipeline (3) is 80mm, and the diameter of the fourth section of pipeline (4) is 100mm.
(2) Chilled brine is introduced into the jacket (5) of the pipe crystallization reactor through a brine inlet, and the flow rate is 6m 3 And (h) pumping the ethanol solution after high-temperature boiling into a pipeline crystallization reactor through a feed inlet, wherein the feed flow rate is 0.8m 3 And (h) cooling through a 4-stage pipeline, and then performing solid-liquid separation through a filter;
(3) And discharging the solid crystals obtained by solid-liquid separation from a discharge hole, drying, discharging the liquid from an inclined pipeline, and purifying and recycling.
Example 2
A maltol pipeline crystallization process comprising the steps of:
(1) Providing a pipeline crystallization reactor, wherein the pipeline crystallization reactor is divided into 4 sections of pipelines and a filter (6);
the top of a first section of pipeline (1) in the 4 sections of pipelines is provided with a feed inlet, a fourth section of pipeline (4) is connected with a filter (6), and the bottom of the filter (6) is provided with a discharge outlet (8);
an inclined pipeline is arranged at the position, close to the discharge hole (7), of the filter (6) to discharge filtrate; a jacket (5) is arranged outside the 4-section pipeline, a brine outlet is arranged at the position, close to the feed inlet (7), of the jacket (5), a brine inlet is arranged at the position, close to the filter (6), of the jacket (5), and the brine temperature is-20 ℃;
the pipe diameter of the 4-section pipeline is as follows: the diameter of the first section of pipeline (1) is 48mm, the diameter of the second section of pipeline (2) is 62mm, the diameter of the third section of pipeline (3) is 78mm, and the diameter of the fourth section of pipeline (4) is 95mm.
(2) Chilled brine is introduced into the jacket (5) of the pipe crystallization reactor through a brine inlet, and the flow rate is 5m 3 And (h) pumping the ethanol solution after high-temperature boiling into a pipeline crystallization reactor through a feed inlet, wherein the feed flow rate is 0.4m 3 And (h) cooling through a 4-stage pipeline, and then performing solid-liquid separation through a filter;
(3) And discharging the solid crystals obtained by solid-liquid separation from a discharge hole, then feeding the solid crystals into a fluidized bed by a conveying belt for drying, discharging the liquid from an inclined pipeline, and then purifying and recycling the liquid.
Example 3
A maltol pipeline crystallization process comprising the steps of:
(1) Providing a pipeline crystallization reactor, wherein the pipeline crystallization reactor is divided into 4 sections of pipelines and a filter (6);
the top of a first section of pipeline (1) in the 4 sections of pipelines is provided with a feed inlet, a fourth section of pipeline (4) is connected with a filter (6), and the bottom of the filter (6) is provided with a discharge outlet (8);
an inclined pipeline is arranged at the position, close to the discharge hole (7), of the filter (6) to discharge filtrate; a jacket (5) is arranged outside the 4-section pipeline, a brine outlet is arranged at the position, close to the feed inlet (7), of the jacket (5), a brine inlet is arranged at the position, close to the filter (6), of the jacket (5), and the brine temperature is-20 ℃;
the pipe diameter of the 4-section pipeline is as follows: the diameter of the first section of pipeline (1) is 52mm, the diameter of the second section of pipeline (2) is 65mm, the diameter of the third section of pipeline (3) is 82mm, and the diameter of the fourth section of pipeline (4) is 100mm.
(2) Chilled brine is introduced into the jacket (5) of the pipe crystallization reactor through a brine inlet, and the flow rate is 8m 3 And (h) pumping the ethanol solution after high-temperature boiling into a pipeline crystallization reactor through a feed inlet, wherein the feed flow rate is 1m 3 And (h) cooling through a 4-stage pipeline, and then performing solid-liquid separation through a filter;
(3) And discharging the solid crystals obtained by solid-liquid separation from a discharge hole, drying, discharging the liquid from an inclined pipeline, and purifying and recycling.
Comparative example 1
A maltol pipeline crystallization process comprising the steps of:
(1) A pipeline crystallization reactor is arranged, the pipeline crystallization reactor is divided into 4 sections of pipelines and a filter,
a feed inlet is formed in the top of a first section of pipeline in the 4 sections of pipelines, a fourth section of pipeline is connected with a filter, and a discharge outlet is formed in the bottom of the filter;
an inclined pipeline is arranged at the position, close to the discharge hole, of the filter to discharge filtrate; a jacket is arranged outside the 4-section pipeline, a brine outlet is arranged at the position of the jacket close to the feed inlet, a brine inlet is arranged at the position of the jacket close to the filter, and the brine temperature is-20 ℃;
the pipe diameter of the 4-section pipeline is as follows: the diameter of the first section of pipeline is 50mm, the diameter of the second section of pipeline is 65mm, the diameter of the third section of pipeline is 80mm, and the diameter of the fourth section of pipeline is 100mm.
(2) Passing chilled brine through brineThe inlet is led into the jacket of the pipe crystallization reactor, the flow velocity is 4m 3 And (h) pumping the ethanol solution after high-temperature boiling into a pipeline crystallization reactor through a feed inlet, wherein the feed flow rate is 1.2m 3 And (h) cooling through a 4-stage pipeline, and then performing solid-liquid separation through a filter;
(3) And discharging the solid crystals obtained by solid-liquid separation from a discharge hole, drying, discharging the liquid from an inclined pipeline, and purifying and recycling.
Comparative example 2
A maltol pipeline crystallization process comprising the steps of:
(1) A pipeline crystallization reactor is arranged, the pipeline crystallization reactor is divided into 4 sections of pipelines and a filter,
a feed inlet is formed in the top of a first section of pipeline in the 4 sections of pipelines, a fourth section of pipeline is connected with a filter, and a discharge outlet is formed in the bottom of the filter;
an inclined pipeline is arranged at the position, close to the discharge hole, of the filter to discharge filtrate; a jacket is arranged outside the 4-section pipeline, a brine outlet is arranged at the position of the jacket close to the feed inlet, a brine inlet is arranged at the position of the jacket close to the filter, and the brine temperature is-20 ℃;
the pipe diameter of the 4-section pipeline is as follows: the diameter of the first section of pipeline is 50mm, the diameter of the second section of pipeline is 65mm, the diameter of the third section of pipeline is 80mm, and the diameter of the fourth section of pipeline is 100mm.
(2) Chilled brine is introduced into the jacket of the pipe crystallization reactor through a brine inlet, and the flow rate is 9m 3 And (h) pumping the ethanol solution after high-temperature boiling into a pipeline crystallization reactor through a feed inlet, wherein the feed flow rate is 1.2m 3 And (h) cooling through a 4-stage pipeline, and then performing solid-liquid separation through a filter;
(3) And discharging the solid crystals obtained by solid-liquid separation from a discharge hole, drying, discharging the liquid from an inclined pipeline, and purifying and recycling.
Comparative example 3
A maltol pipeline crystallization process comprising the steps of:
(1) A pipeline crystallization reactor is arranged, the pipeline crystallization reactor is divided into a pipeline and a filter,
the top of the pipeline is provided with a feed inlet, and the bottom of the filter is provided with a discharge outlet;
an inclined pipeline is arranged at the position, close to the discharge hole, of the filter to discharge filtrate;
a jacket is arranged outside the pipeline;
a brine outlet is arranged at the position of the jacket close to the feed inlet, a brine inlet is arranged at the position of the jacket close to the filter, and the brine temperature is-20 ℃;
the pipe diameter of the pipeline is as follows: 100mm.
(2) Chilled brine is introduced into the jacket of the pipe crystallization reactor through a brine inlet, and the flow rate is 6m 3 And (h) pumping the ethanol solution after high-temperature boiling into a pipeline crystallization reactor through a feed inlet, wherein the feed flow rate is 0.8m 3 And/h, cooling through a pipeline, and then performing solid-liquid separation through a filter;
(3) And discharging the solid crystals obtained by solid-liquid separation from a discharge hole, drying, discharging the liquid from an inclined pipeline, and purifying and recycling.
Comparative example 4
A maltol pipeline crystallization process comprising the steps of:
(1) A pipeline crystallization reactor is arranged, the pipeline crystallization reactor is divided into a pipeline and a filter,
the top of the pipeline is provided with a feed inlet, and the bottom of the filter is provided with a discharge outlet;
an inclined pipeline is arranged at the position, close to the discharge hole, of the filter to discharge filtrate;
a jacket is arranged outside the pipeline;
a brine outlet is arranged at the position of the jacket close to the feed inlet, a brine inlet is arranged at the position of the jacket close to the filter, and the brine temperature is-20 ℃;
the pipe diameter of the pipeline is as follows: 50mm.
(2) Chilled brine is introduced into the jacket of the pipe crystallization reactor through a brine inlet, and the flow rate is 6m 3 And (h) pumping the ethanol solution after high-temperature boiling into a pipeline crystallization reactor through a feed inlet, wherein the feed flow rate is 0.8m 3 And/h, cooling through a pipeline, and then performing solid-liquid separation through a filter;
(3) And discharging the solid crystals obtained by solid-liquid separation from a discharge hole, drying, discharging the liquid from an inclined pipeline, and purifying and recycling.
Comparative example 5
The two-step kettle cooling crystallization method comprises the following steps:
after the sublimated product is put into the material boiling kettle, a material feeding cover is arranged, ethanol is put into the kettle from a material mixing groove, stirring and steam are started, the steam pressure is controlled after the mixture flows back, and when the temperature is increased to be less than or equal to 85 ℃, the steam is turned off and stirring is performed. And (3) discharging the materials to a water cooling kettle, stirring, cooling the materials with circulating water to be less than or equal to 45 ℃, and cooling the materials in a freezing kettle. Freezing and crystallizing: stirring after the materials are put into a freezing kettle, starting to cool by opening a salt water valve, cooling to less than or equal to 10 ℃, discharging the materials into a centrifuge for spin-drying, centrifuging out ethanol for recycling, weighing and recording wet finished products, and drying.
Results
The crystallization yields and the crystal grain size distribution of the crystallization methods of the respective examples were counted, and the results are counted in table 1.
Table 1 crystallization yields and grain size distribution of crystalline particles according to the methods of examples
The result shows that compared with the two-step kettle cooling crystallization method, the pipeline crystallization method can adjust the residence time of the material in the pipe diameter by controlling the material flow rate and the pipe diameter of the pipeline crystallization reactor, thereby achieving the purpose of sufficiently and quickly cooling, improving the crystallization yield by more than 5 percent, improving the production efficiency and finally obtaining better crystal particles.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present utility model. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present utility model is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present utility model.
Claims (10)
1. A pipeline crystallization reactor is characterized by comprising 4 sections of pipelines and a filter,
a feed inlet is formed in the top of a first section of pipeline in the 4 sections of pipelines, a fourth section of pipeline is connected with a filter, and a discharge outlet is formed in the bottom of the filter;
an inclined pipeline is arranged at the position, close to the discharge hole, of the filter to discharge filtrate;
the outside of the 4 sections of pipelines is provided with a jacket, a brine outlet is arranged at the position of the jacket close to the feed inlet, and a brine inlet is arranged at the position of the jacket close to the filter.
2. The pipe crystallization reactor according to claim 1, wherein the pipe diameter of the 4-stage pipe is: the diameter of the first section of pipeline is 48-52mm, the diameter of the second section of pipeline is 62-65mm, the diameter of the third section of pipeline is 78-82mm, and the diameter of the fourth section of pipeline is 95-100mm.
3. The pipe crystallization reactor according to claim 2, wherein the pipe diameter of the 4-stage pipe is: the diameter of the first section of pipeline is 50mm, the diameter of the second section of pipeline is 65mm, the diameter of the third section of pipeline is 80mm, and the diameter of the fourth section of pipeline is 100mm.
4. Use of a pipe crystallization reactor according to any one of claims 1-3 for the production of maltol.
5. A process for the crystallization of maltol in a pipeline, comprising the steps of:
(1) Introducing frozen brine into the jacket of the pipeline crystallization reactor according to any one of claims 1-3 through a brine inlet, then pumping the ethanol solution after high-temperature boiling into the pipeline crystallization reactor through a feed inlet, cooling through a 4-stage pipeline, and performing solid-liquid separation through a filter;
(2) And discharging the solid crystals obtained by solid-liquid separation from a discharge hole, drying, discharging the liquid from an inclined pipeline, and purifying and recycling.
6. The method of claim 5, wherein the chilled brine has a temperature of-15 to-25 ℃.
7. The method according to claim 5, wherein the flow rate of the frozen brine is 5-8m 3 /h。
8. The method according to claim 5, wherein the ethanol solution after high-temperature boiling is a product obtained by adding ethanol into a product obtained by a sublimation section in the production process of maltol.
9. The method according to claim 5, wherein the ethanol solution is fed at a flow rate of 0.4-1m 3 /h。
10. The method according to claim 9, wherein the feed flow rate of the ethanol solution is 0.8m 3 /h。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311396158.0A CN117504345A (en) | 2023-10-25 | 2023-10-25 | Novel maltol pipeline crystallization process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311396158.0A CN117504345A (en) | 2023-10-25 | 2023-10-25 | Novel maltol pipeline crystallization process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117504345A true CN117504345A (en) | 2024-02-06 |
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| CN202311396158.0A Pending CN117504345A (en) | 2023-10-25 | 2023-10-25 | Novel maltol pipeline crystallization process |
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