CN112479228A - Refining device and method for ammonium chloride crude product in sucralose chlorination neutralization and salt pressing working section - Google Patents

Refining device and method for ammonium chloride crude product in sucralose chlorination neutralization and salt pressing working section Download PDF

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Publication number
CN112479228A
CN112479228A CN202011367933.6A CN202011367933A CN112479228A CN 112479228 A CN112479228 A CN 112479228A CN 202011367933 A CN202011367933 A CN 202011367933A CN 112479228 A CN112479228 A CN 112479228A
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hydrogen peroxide
kettle
mother liquor
decoloring
ammonium chloride
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CN202011367933.6A
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赵金刚
钱庆喜
周万全
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Anhui Jinhe Industrial Co Ltd
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Anhui Jinhe Industrial Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/16Halides of ammonium
    • C01C1/164Ammonium chloride

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to a refining device and a method for ammonium chloride crude products in a sucralose chlorination neutralization salt pressing working section, which are characterized by comprising the following steps: (1) pumping the centrifugal mother liquor in the mother liquor head tank into a hydrogen peroxide decoloring kettle, adding hydrogen peroxide into the hydrogen peroxide decoloring kettle, and controlling the volume ratio of the mother liquor to the hydrogen peroxide to be (95-105): 1, (2) controlling the temperature in the hydrogen peroxide decoloring kettle to be 30-60 ℃, circulating the materials in the hydrogen peroxide decoloring kettle for 25-35min, heating the materials to 60-70 ℃ through a pipeline, and then sending the materials into a dissolving kettle. The invention has the advantages that: the original decoloring technology is improved, and after the decoloring treatment by hydrogen peroxide, the color of the product is obviously improved, and the content of ammonium chloride nitrogen is also improved to more than 24.5 percent; the recovery rate is increased while the product quality is improved, the problem of solid waste treatment generated in the production of sucralose is well solved, and the method has strong environmental protection benefits and economic benefits.

Description

Refining device and method for ammonium chloride crude product in sucralose chlorination neutralization and salt pressing working section
Technical Field
The invention belongs to the technical field of sucralose production, and relates to a refining device and a refining method for ammonium chloride crude products in sucralose chlorination neutralization salt pressing working sections.
Background
Sucralose is used as a novel sweet food additive, has more advantages than sucrose, saccharin, AK sugar, aspartame, stevioside and the like, has high safety and stable performance, is a novel high-quality non-nutritional high-efficiency sweetener, and is an optimal ideal sweet substitute for foods for patients with obesity, cardiovascular diseases and diabetes mellitus; also belongs to the field of fine chemical products, and is a branch product of food additives. It has not only rapidly expanded application range in health food and medicine, but also widely applied to more than 300 processed products such as baked food, beverage, chewing coffee, dairy product, frozen dessert, ice cream, pudding, jelly, jam, syrup and the like, has been widely accepted by the market at present and becomes one of the most popular high-potency sweeteners
In the production process of sucralose, the ammonium chloride crude product generated by centrifugation in the neutralization and salt pressing section contains about 60% of ammonium chloride salt, and because the ammonium chloride crude product contains organic tin, DMF, polychlorinated sugar and other substances, the content and color of the ammonium chloride product cannot reach high quality, and the ammonium chloride product is low in price for direct sale.
Disclosure of Invention
The invention aims to solve the problems of low quality (low content, impure color and the like), low selling price and poor economic benefit of the ammonium chloride crude product produced in the prior art, and provides a device and a method for refining the ammonium chloride crude product in a sucralose chlorination neutralization and salt pressing section.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a refining plant for ammonium chloride crude products in sucralose chlorination neutralization salt pressing section comprises the following existing equipment: mother liquor groove elevated tank, solution cauldron, pressure filter, wash bowl, cooling cauldron, crystallization kettle, centrifuge, centrifugation mother liquor groove, its characterized in that: a hydrogen peroxide decoloring kettle is additionally arranged between the mother liquid head tank and the material dissolving kettle; the mother liquid elevated tank is connected with the top inlet of the hydrogen peroxide decoloring kettle through a pipeline, and the bottom outlet of the hydrogen peroxide decoloring kettle is connected with the top inlet of the dissolving kettle through a pipeline, a pump and a heater; the hydrogen peroxide head tank is connected to the inlet of the hydrogen peroxide decoloring kettle through a pipeline, and the bottom of the hydrogen peroxide decoloring kettle is connected to the top inlet of the hydrogen peroxide decoloring kettle through a pipeline, a pump and a condenser.
A method for refining ammonium chloride crude product in sucralose chlorination neutralization salt pressing working section comprises the following working sections: dissolving, filter pressing, washing, cooling, crystallizing and centrifuging, and is characterized by comprising the following steps:
(1) pumping the mother liquor (from a centrifugal working section) in the high-level tank of the mother liquor tank into a hydrogen peroxide decoloring kettle, adding hydrogen peroxide into the hydrogen peroxide decoloring kettle, and controlling the volume ratio of the mother liquor to the hydrogen peroxide to be 95-105: 1;
(2) controlling the temperature in the hydrogen peroxide decoloring kettle to be 30-60 ℃, circulating the materials in the hydrogen peroxide decoloring kettle for 25-35min, heating the materials to 60-70 ℃ through a pipeline, and then sending the materials into a dissolving kettle.
The invention utilizes the strong oxidizing property of hydrogen peroxide to decolorize the solution of the crude ammonium chloride product, and after heat preservation, the solution is cooled after impurities are removed by a filter press; when the temperature reaches within 45 ℃, a centrifugal machine is used for centrifugal operation to refine the ammonium chloride into refined ammonium chloride products, so as to reduce the production cost of the sucralose and enhance the product competitiveness.
The invention has the advantages that: the original decoloring technology is improved, most of impurities are filtered and removed by a filter press after the decoloration treatment by hydrogen peroxide, so that the color of the product is obviously improved, and the content of ammonium chloride is greatly improved (more than 85 percent); through data comparison in experiments, the recovery rate is increased while the product quality is improved, the problem of solid waste treatment in sucralose production is well solved, and the method has strong environmental protection benefits and economic benefits (see the following table).
Figure DEST_PATH_IMAGE002
Drawings
FIG. 1 is a schematic process flow diagram of the present invention;
FIG. 2 is a schematic diagram of a conventional process.
Detailed Description
The invention is further illustrated with reference to fig. 1:
a refining plant for ammonium chloride crude products in sucralose chlorination neutralization salt pressing section comprises the following equipment: the mother liquid elevated tank is connected with a top inlet of the hydrogen peroxide decoloring kettle through a pipeline, a bottom outlet of the hydrogen peroxide decoloring kettle is connected with a top inlet of the dissolving kettle through a pipeline, a pump and a heater, a bottom outlet of the dissolving kettle is sequentially connected with the filter press, the cooling kettle, the crystallization kettle, the centrifuge, the centrifugal mother liquid tank and the mother liquid tank through pipelines, and an outlet of the mother liquid tank is connected to an inlet of the mother liquid elevated tank through a pipeline; wherein, the outlet at the bottom of the hydrogen peroxide decoloring kettle is connected with the inlet at the top of the hydrogen peroxide decoloring kettle through a pipeline, a pump and a cooler, a pipeline is added on the outlet pipeline of the filter press and connected with the inlet at the top of the rinsing bath, and the outlet at the bottom of the rinsing bath is connected with the inlet pipeline of the filter press through a pipeline and a pump.
A method for refining ammonium chloride crude product in sucralose chlorination neutralization salt pressing section comprises the following specific implementation steps:
example 1
(1) 3500L of mother liquor (from a centrifugal section) is put into a hydrogen peroxide decoloring kettle from a mother liquor head tank, and 18kg of hydrogen peroxide is dripped into the hydrogen peroxide decoloring kettle (heat is released in the dripping process);
(2) opening a circulating pump of the hydrogen peroxide decoloring kettle, cooling the circulating pump by using a condenser, controlling the temperature in the hydrogen peroxide decoloring kettle to be 50-53 ℃, and keeping the temperature in the hydrogen peroxide decoloring kettle stable;
(3) after the dropwise adding is finished, a decoloring kettle feeding pump is used for feeding the materials into a dissolving kettle, and the materials are heated to 60 ℃ by a heater in the process of feeding the materials into the dissolving kettle;
(4) 750kg of crude ammonium chloride product is added into the material dissolving kettle, and 10kg of active carbon is added into the material dissolving kettle; heating the material dissolving kettle to 85 ℃, and preserving heat for 1 hour;
(5) after the heat preservation is finished, the solution in the dissolving kettle is sent to a filter press for filtering and removing impurities, the filtrate is then sent to a cooling kettle for cooling, and when the temperature in the cooling kettle is lower than 50 ℃, the material is put into a crystallization kettle for crystallization;
(6) when the temperature in the crystallization kettle is lower than 40 ℃, centrifuging the materials in the crystallization kettle, packaging the centrifuged crystals (fine ammonium chloride), feeding the centrifuged filtrate into a centrifugal mother liquor tank, and then sequentially pumping into a mother liquor tank and a mother liquor tank head tank.
The quality of the ammonium chloride finished product obtained by the method reaches the top grade, and the nitrogen content is higher (24.8%); the thrown mother liquor can be used mechanically to reduce the discharge of waste water.
Example 2
(1) 3500L of mother liquor (from a centrifugal section) is put into the hydrogen peroxide decoloring kettle from the head tank of the mother liquor tank, and 15kg of hydrogen peroxide is dripped into the hydrogen peroxide decoloring kettle;
(2) opening a circulating pump of the hydrogen peroxide decoloring kettle, cooling the circulating pump by using a condenser, controlling the temperature in the hydrogen peroxide decoloring kettle to be 55-58 ℃, and keeping the temperature in the hydrogen peroxide decoloring kettle stable;
(3) after the dropwise adding is finished, a decoloring kettle feeding pump is used for feeding the materials into a dissolving kettle, and the materials are heated to 60 ℃ by a heater in the process of feeding the materials into the dissolving kettle;
(4) 750kg of crude ammonium chloride product is added into the material dissolving kettle, and 10kg of active carbon is added into the material dissolving kettle; heating the material dissolving kettle to 90 ℃, and preserving heat for 1 hour;
(5) after the heat preservation is finished, the solution in the dissolving kettle is sent to a filter press for filtering and removing impurities, the filtrate is then sent to a cooling kettle for cooling, and when the temperature in the cooling kettle is lower than 50 ℃, the material is put into a crystallization kettle for crystallization;
(6) and when the temperature in the crystallization kettle is lower than 40 ℃, centrifuging the materials in the crystallization kettle, packaging the centrifuged crystals (crude ammonium chloride), feeding the centrifuged filtrate into a centrifugal mother liquor tank, and then sequentially pumping into a mother liquor tank and a mother liquor tank head tank.
The quality of the ammonium chloride finished product obtained by the method reaches the top grade, and the nitrogen content is higher (25.1%); the thrown mother liquor can be used mechanically to reduce the discharge of waste water.
Example 3
(1) 3500L of mother liquor (from a centrifugal section) is put into the hydrogen peroxide decoloring kettle from the head tank of the mother liquor tank, and 20kg of hydrogen peroxide is dripped into the hydrogen peroxide decoloring kettle;
(2) opening a circulating pump of the hydrogen peroxide decoloring kettle, cooling the circulating pump by using a condenser, controlling the temperature in the hydrogen peroxide decoloring kettle to be 33-35 ℃, and keeping the temperature in the hydrogen peroxide decoloring kettle stable;
(3) after the dropwise adding is finished, a decoloring kettle feeding pump is used for feeding the materials into a dissolving kettle, and the materials are heated to 60 ℃ by a heater in the process of feeding the materials into the dissolving kettle;
(4) 750kg of crude ammonium chloride product is added into the material dissolving kettle, and 10kg of active carbon is added into the material dissolving kettle; heating the material dissolving kettle to 95 ℃, and preserving heat for 1 hour;
(5) after the heat preservation is finished, the solution in the dissolving kettle is sent to a filter press for filtering and removing impurities, the filtrate is then sent to a cooling kettle for cooling, and when the temperature in the cooling kettle is lower than 50 ℃, the material is put into a crystallization kettle for crystallization;
(6) and when the temperature in the crystallization kettle is lower than 40 ℃, centrifuging the materials in the crystallization kettle, packaging the centrifuged crystals (crude ammonium chloride), feeding the centrifuged filtrate into a centrifugal mother liquor tank, and then sequentially pumping into a mother liquor tank and a mother liquor tank head tank.
The quality of the ammonium chloride finished product obtained by the method reaches the top grade, and the nitrogen content is higher (24.9%); the thrown mother liquor can be used mechanically to reduce the discharge of waste water.

Claims (2)

1. A refining plant for ammonium chloride crude products in sucralose chlorination neutralization salt pressing section comprises the following existing equipment: mother liquor groove elevated tank, solution cauldron, pressure filter, wash bowl, cooling cauldron, crystallization kettle, centrifuge, centrifugation mother liquor groove, its characterized in that: a hydrogen peroxide decoloring kettle is additionally arranged between the mother liquid head tank and the material dissolving kettle; the mother liquid tank elevated tank is connected with the top inlet of the hydrogen peroxide decoloring kettle through a pipeline, and the bottom outlet of the hydrogen peroxide decoloring kettle is connected with the top inlet of the dissolving kettle through a pipeline, a pump and a heater; the hydrogen peroxide head tank is connected to the inlet of the hydrogen peroxide decoloring kettle through a pipeline, and the bottom of the hydrogen peroxide decoloring kettle is connected to the top inlet of the hydrogen peroxide decoloring kettle through a pipeline, a pump and a condenser.
2. A method for refining ammonium chloride crude product in sucralose chlorination neutralization salt pressing working section comprises the following working sections: dissolving, filter pressing, washing, cooling, crystallizing and centrifuging, and is characterized by comprising the following steps:
(1) pumping the mother liquor in the mother liquor tank head tank into a hydrogen peroxide decoloring kettle, adding hydrogen peroxide into the hydrogen peroxide decoloring kettle, and controlling the volume ratio of the mother liquor to the hydrogen peroxide to be 95-105: 1,
(2) controlling the temperature in the hydrogen peroxide decoloring kettle to be 30-60 ℃, circulating the materials in the hydrogen peroxide decoloring kettle for 25-35min, heating the materials to 60-70 ℃ through a pipeline, and then sending the materials into a dissolving kettle.
CN202011367933.6A 2020-11-30 2020-11-30 Refining device and method for ammonium chloride crude product in sucralose chlorination neutralization and salt pressing working section Pending CN112479228A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1122611A1 (en) * 1982-09-16 1984-11-07 Belov Vikentij N Method for purifying ammonium chloride
CN102826673A (en) * 2011-06-15 2012-12-19 浙江龙盛化工研究有限公司 Cleaning treatment method of dying industrial acidic wastewater
CN106145490A (en) * 2015-05-12 2016-11-23 刘风鸣 A kind of expoxy propane calcium chloride saponification waste-water processes method of resource
CN108249460A (en) * 2018-01-13 2018-07-06 安徽金禾实业股份有限公司 In a kind of Sucralose and the processing method of press filtration workshop section ammonium chloride waste residue
CN109422399A (en) * 2017-08-28 2019-03-05 中国石油化工股份有限公司 The processing method of ammonium salt-containing waste water
CN109608417A (en) * 2018-10-24 2019-04-12 科迈化工股份有限公司 Method by recycling the direct synthesis accelerant MBTS of crude product MBT in resin
CN210855657U (en) * 2019-09-27 2020-06-26 广东中耀环境科技有限公司 Waste liquid treatment device

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1122611A1 (en) * 1982-09-16 1984-11-07 Belov Vikentij N Method for purifying ammonium chloride
CN102826673A (en) * 2011-06-15 2012-12-19 浙江龙盛化工研究有限公司 Cleaning treatment method of dying industrial acidic wastewater
CN106145490A (en) * 2015-05-12 2016-11-23 刘风鸣 A kind of expoxy propane calcium chloride saponification waste-water processes method of resource
CN109422399A (en) * 2017-08-28 2019-03-05 中国石油化工股份有限公司 The processing method of ammonium salt-containing waste water
CN108249460A (en) * 2018-01-13 2018-07-06 安徽金禾实业股份有限公司 In a kind of Sucralose and the processing method of press filtration workshop section ammonium chloride waste residue
CN109608417A (en) * 2018-10-24 2019-04-12 科迈化工股份有限公司 Method by recycling the direct synthesis accelerant MBTS of crude product MBT in resin
CN210855657U (en) * 2019-09-27 2020-06-26 广东中耀环境科技有限公司 Waste liquid treatment device

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Application publication date: 20210312