CN1803582A - Method and apparatus for continuous production of high-concentrated sodium hypochlorite - Google Patents

Method and apparatus for continuous production of high-concentrated sodium hypochlorite Download PDF

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Publication number
CN1803582A
CN1803582A CN 200610020231 CN200610020231A CN1803582A CN 1803582 A CN1803582 A CN 1803582A CN 200610020231 CN200610020231 CN 200610020231 CN 200610020231 A CN200610020231 A CN 200610020231A CN 1803582 A CN1803582 A CN 1803582A
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sodium hypochlorite
chlorination kettle
salt
settling
kettle
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CN100453449C (en
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罗云
李强
袁雄
陈华
孙永贵
覃仁莲
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Yibin Tianyuan Group Co Ltd
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Yibin Tianyuan Group Co Ltd
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Abstract

The invention discloses a method to continual produce high-concentration sodium hypochlorite, which comprises: generating sodium hypochlorite solution, depositing for desalinization, and discharging salt. Wherein, the opposite device comprises a chloridization kettle inserted with two groups of inlet chlorine pipes, a group of subsiders in series, a salt mud tank, and a centrifuge. Wherein, the reaction kettle comprises a reaction area and a deposition area; forcing the qualified sodium hypochlorite supernatant into deposition slot through overflow port. This invention can keep the liquid level invariable and production continual, and has no pollution to environment.

Description

Method and device for continuously producing high-concentration sodium hypochlorite
Technical Field
The invention relates to a method for continuously producing high-concentration sodium hypochlorite by using sodium hydroxide and chlorine.
Background
Sodium hypochlorite, a chemical formula of NaClO, is a yellow extremely unstable solid, is dissolved in water, and an aqueous solution is in an alkaline reaction and can be gradually decomposed into sodium chloride, sodium chlorate and oxygen. The strong oxidant is widely used for bleaching paper pulp and fabrics, is used as an oxidant and a water purifying agent, and is also a main raw material for producing hydrazine hydrate.
The conventional process for producing low-concentration sodium hypochlorite by using dilute alkali as a raw material and adding chlorine gas comprises the steps of introducing the chlorine gas into a chlorination kettle containing 25% sodium hydroxide solution, and reacting at the temperature lower than 15 ℃ to generate sodium hypochlorite and sodium chloride, wherein the effective chlorine content of the produced sodium hypochlorite is 60g/l, the free alkali content is 145g/l, and the by-product sodium chloride cannot be separated out due to low concentration and exists in the sodium hypochlorite solution to influence the quality and performance of the sodium hypochlorite solution; meanwhile, the conventional process is intermittent production, the yield of the sodium hypochlorite single kettleis low, large-scale continuous production cannot be realized by the process, the labor intensity is increased, and production equipment is added.
Unfortunately, no production plant can produce high-concentration sodium hypochlorite in industry, and the continuous production of the high-concentration sodium hypochlorite cannot be realized at the root because the technical problems of continuous chlorine gas introduction and salt scale removal cannot be solved well. From the reaction mechanism, the conventional single-tube chlorine feeding mode often causes the phenomenon of local over-chlorination reaction and sodium hypochlorite decomposition due to uneven distribution of chlorine, which has great influence on the quality of sodium hypochlorite products, and simultaneously produces high-concentration sodium hypochlorite, a large amount of by-product sodium chloride can be separated out, if a salt scale removing technology is not available, the blockage of a chlorine feeding pipeline is caused, so that the continuous production of the sodium hypochlorite cannot be ensured, and in addition, if the large amount of separated by-product sodium chloride is not discharged in time, the continuous production cannot be ensured; and the byproduct sodium chloride can not be effectively used, which causes environmental pollution and waste of byproduct resources.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for continuously producing sodium hypochlorite with high concentration, wherein the effective chlorine of the sodium hypochlorite is controlled to be more than or equal to 130g/l and the free alkali content is more than or equal to 40g/1 in a large scale; the invention also aims to provide equipment for continuously producing the high-concentration sodium hypochlorite.
The purpose of the invention is realized as follows:
a method for continuously producing high-concentration sodium hypochlorite comprises the following steps:
a. generation of sodium hypochlorite solution: introducing chlorine gas into a chlorination kettle containing 30% sodium hydroxide solution, reacting at a temperature lower than 15 ℃ to generate sodium hypochlorite and sodium chloride, when the content of sodium hypochlorite effective chlorine in the reaction liquid is more than or equal to 130g/l and the content of free alkali is more than or equal to 40g/l, continuously adding the 30% sodium hydroxide solution into the reaction liquid and continuously introducing the chlorine gas, and simultaneously ensuring that the content of the sodium hypochlorite effective chlorine in the reaction liquid in the chlorination kettle is more than or equal to 130g/l and the content of the free alkali is more than or equal to 40 g/l;
b. settling and desalting: overflowing reaction liquid in the chlorination kettle into a settling tank for continuous settling, separating to obtain a sodium hypochlorite solution with the concentration of more than 23% of sodium hypochlorite and the content of sodium chloride lower than 125g/l, enriching the separated sodium chloride in the settling tank to a certain degree, and then periodically discharging the sodium chloride into a salt mud tank;
c. discharging salt from a chlorination kettle: and (3) discharging the sodium chloride settled at the bottom in the chlorination kettle into a salt mud tank from the bottom in the chlorination kettle at regular intervals.
Wherein, the invention can also add the step of recovering salt by centrifugation: namely, the sodium chloride in the salt mud tank is centrifugally separated to obtain solid sodium chloride and centrifugal mother liquor, the separated centrifugal mother liquor is returned to a chlorination kettle for use, and the separated solid sodium chloride is used for preparing brine.
Apparatus for use in the method of the invention, comprising:
the chlorination kettle is a reactor which is formed by a shell, wherein the upper half part of the reactor is a reaction zone and the lower half part of the reactor is a settling zone, and two groups of parallel chlorine pipes are inserted into the bottom area in the chlorination kettle from the upper opening of the chlorination kettle;
a set of settling tanks connected in series, wherein the first settling tank is communicated with the chlorination kettle through an overflow pipe;
and the salt mud tank is arranged at the lower part of the chlorination kettle, is communicated with the outlet of the settling area of the chlorination kettle through a pipeline and is communicated with the last settling tank through a pipeline.
Wherein, a centrifuge can be added and is communicated with the salt discharge port of the salt mud tank through a salt discharge pipeline.
Compared with the prior art, the invention has the following advantages:
introducing chlorine; the mode of filling chlorine by inserting the chlorine into the bottom of the kettle by uniformly distributing the chlorine-filling coil pipes on the top of the kettle replaces the mode of filling chlorine by a single pipe, thereby solving the phenomena of local over-chlorination reaction and sodium hypochlorite decomposition caused by uneven distribution of chlorine. The invention adopts the mode of inserting bottom and leading chlorine, belongs to chemical absorption, and the tail gas after reaction enters the tail gas treatment system, so the system almost has no tail gas emission and can not cause pollution to the environment;
continuity: the chlorination kettle is provided with two groups of chlorine introducing pipes, when one group of chlorine introducing pipes is blocked and dredged, the other group of chlorine introducing pipes continues to introduce chlorine gas for reaction, and the continuity of production is ensured. The reaction kettle is divided into a reaction area and a settling area, qualified sodium hypochlorite clear liquid enters the settling tank through the overflow port, the liquid level in the kettle is kept constant, and the production continuity is guaranteed.
And (3) separating sodium chloride: the salt mud in the settling zone of the reaction kettle is discharged at regular time and enters a settling tank, the clear liquid after secondary settling enters a storage tank, the salt mud enters a centrifugal machine for centrifugal separation, and the centrifugal mother liquid returns to the chlorination kettle to be beneficial to the growth of salt grains in the kettle and the recycling of centrifugal salt.
The effective chlorine of sodium hypochlorite is increased to more than 130g/l from 50g/l, so that salt can be fully separated out, the solid NaCl is separated by a titanium centrifuge, 15000 tons of sodium hypochlorite with the annual concentration of more than 23 percent can be produced, 10000 tons of solid salt can be recovered, and the centrifugal mother liquor returns to the chlorination kettle to be beneficial to the growth of salt particles.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a view showing the structure of the apparatus of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited to these examples.
Example 1: a method for continuously producing high-concentration sodium hypochlorite comprises the following steps:
a. generation of sodium hypochlorite solution: firstly, before starting up, a 30% sodium hydroxide solution is pumped into an alkali distribution table by a pump and enters a chlorination kettle by controlling the flow through a flow meter, when the sodium hydroxide solution of the chlorination kettle reaches the liquid level of 2.5-2.7, a stirring motor of the chlorination kettle is started, alkali feeding is stopped, frozen brine is conveyed to a coil pipe in the kettle, when the temperature of materials in the chlorination kettle is lower than 15 ℃, chlorine gas is introduced into the chlorination kettle by controlling the flow of the chlorine gas through a rotor flow meter, so that the sodium hydroxide and the chlorine gas react, and the chemical reaction equation is as follows:
when the available chlorine of sodium hypochlorite in the chlorination kettle is more than or equal to 130g/l and the content of free alkali is more than or equal to 40g/l, starting a concentrated alkali pump to add 30% of sodium hydroxide solution into the chlorination kettle according to a certain flow through a rotor flow meter, and ensuring that the available chlorine of sodium hypochlorite in the kettle is more than or equal to 130g/l and the content of free alkali is more than or equal to 40 g/l.
b. Settling and desalting: overflowing reaction liquid in the chlorination kettle into a settling tank for continuous settling, separating to obtain asodium hypochlorite solution with the concentration of more than 23% of sodium hypochlorite and the content of sodium chloride lower than 125g/l, enriching the separated sodium chloride in the settling tank to a certain degree, and then periodically discharging the sodium chloride into a salt mud tank; the exothermic heat of reaction is removed by the frozen brine.
d. Discharging salt from a chlorination kettle: the sodium chloride settled at the bottom in the chlorination kettle is periodically discharged into a salt mud tank from the bottom in the chlorination kettle, the sodium chloride in the salt mud tank is centrifuged and then enters a salt dissolving system to prepare salt water, and the centrifuged mother liquor enters the chlorination kettle to be beneficial to the growth of salt particles.
Apparatus for use in the method of the invention, comprising:
a chlorination kettle (1) which is a reactor formed by a shell (1-1) and provided with a reaction zone (1-2) at the upper half part and a settling zone (1-3) at the lower half part, wherein two groups of chlorine introducing pipes (1-4) and (1-5) which are arranged in parallel are inserted into the bottom area in the chlorination kettle (1) from the upper opening of the chlorination kettle (1);
a group of settling tanks (2) connected in series, wherein the first settling tank (2) is communicated with the chlorination kettle (1) through an overflow pipe (2-1);
and the salt mud tank (3) is arranged at the lower part of the chlorination kettle (1), is communicated with an outlet (1-6) of a settling area (1-3) of the chlorination kettle (1) through a pipeline (3-1), and is communicated with the last settling tank (2) through a pipeline (3-2).
Wherein, a centrifuge (4) can be added and is communicated with a salt discharge port (3-3) of the salt mud tank (3) through a salt discharge pipeline (4-1).
When the chlorine introducing pipes (1-4) are blocked, the group of chlorine introducing pipes (1-4) is closed, the other group of chlorine introducing pipes (1-5) is opened to continue chlorine introduction, and water is sprayed by a jet pump to automatically dredge the blocked group of chlorine introducing pipes (1-4) for later use.

Claims (6)

1. A method for continuously producing high-concentration sodium hypochlorite is characterized by comprising the following steps:
a. generation of sodium hypochlorite solution: introducing chlorine gas into a chlorination kettle containing 30% sodium hydroxide solution, reacting at a temperature lower than 15 ℃ to generate sodium hypochlorite and sodium chloride, when the content of sodium hypochlorite effective chlorine in the reaction liquid is more than or equal to 130g/l and the content of free alkali is more than or equal to 40g/l, continuously adding the 30% sodium hydroxide solution into the reaction liquid and continuously introducing the chlorine gas, and simultaneously ensuring that the content of the sodium hypochlorite effective chlorine in the reaction liquid in the chlorination kettle is more than or equal to 130g/l and the content of the free alkali is more than or equal to 40 g/l;
b. settling and desalting: overflowing reaction liquid in the chlorination kettle into a settling tank for continuous settling, separating to obtain a sodium hypochlorite solution with the concentration of more than 23% of sodium hypochlorite and the content of sodium chloride lower than 125g/l, enriching the separated sodium chloride in the settling tank to a certain degree, and then periodically discharging the sodium chloride into a salt mud tank;
c. discharging salt from a chlorination kettle: and (3) discharging the sodium chloride settled at the bottom in the chlorination kettle into a salt mud tank from the bottom in the chlorination kettle at regular intervals.
2. The method for continuously producing high-concentration sodium hypochlorite according to claim 1, further comprising a step of recovering salt by centrifugation: namely, the sodium chloride in the salt mud tank is centrifugally separated to obtain solid sodium chloride and centrifugal mother liquor.
3. The method for continuously producing sodium hypochlorite with high concentration according to claim 3, characterized in that the separated centrifugal mother liquor is returned to the chlorination reactor for use.
4. The process for the continuous production of high concentration sodium hypochlorite according to claim 3, characterized in that the separated solid sodium chloride is used to make brine.
5. An apparatus for implementing the method of claim 1, characterized in that the apparatus comprises:
a chlorination kettle (1) which is a reactor formed by a shell (1-1) and provided with a reaction zone (1-2) at the upper half part and a settling zone (1-3) at the lower half part, wherein two groups of chlorine introducing pipes (1-4) and (1-5) which are arranged in parallel are inserted into the bottom area in the chlorination kettle (1) from the upper opening of the chlorination kettle (1);
a group of settling tanks (2) connected in series, wherein the first settling tank (2) is communicated with the chlorination kettle (1) through an overflow pipe (2-1);
and the salt mud tank (3) is arranged at the lower part of the chlorination kettle (1), is communicated with an outlet (1-6) of a settling area (1-3) of the chlorination kettle (1) through a pipeline (3-1), and is communicated with the last settling tank (2) through a pipeline (3-2).
6. The apparatus according to claim 5, characterized by a centrifuge (4) which is connected to the salt discharge opening (3-3) of the salt mud tank (3) via a salt discharge conduit (4-1).
CNB2006100202314A 2006-01-25 2006-01-25 Method and apparatus for continuous production of high-concentrated sodium hypochlorite Active CN100453449C (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102009958A (en) * 2010-12-23 2011-04-13 何卫东 Device and method for producing bleacher from waste chlorine generated in lithium production
CN103241713A (en) * 2013-05-15 2013-08-14 乳源东阳光电化厂 Preparation method of sodium hypochlorite
CN104478151A (en) * 2014-12-18 2015-04-01 重庆海洲化学品有限公司 Environment-friendly treatment method of caustic-soda-containing sodium hypochlorite waste liquor
CN107673311A (en) * 2017-11-30 2018-02-09 山东尚舜化工有限公司 A kind of continuous device and method for preparing the high-concentrated sodium hypochlorite aqueous solution
CN111792625A (en) * 2020-08-26 2020-10-20 河北泽世康环保科技有限公司 Method for producing sodium hypochlorite
CN117742278A (en) * 2024-02-07 2024-03-22 四川飞洁科技发展有限公司 Intelligent monitoring and management method and system for sodium hypochlorite production process

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2532291A1 (en) * 1982-08-24 1984-03-02 Ugine Kuhlmann OBTAINING HIGH-CONCENTRATION SODIUM HYPOCHLORITE SOLUTION BY A CONTINUOUS PROCESS
US5085847A (en) * 1989-05-18 1992-02-04 Olin Corporation Apparatus for producing a fast dissolving granular product
JP2002332585A (en) * 2001-05-10 2002-11-22 Takuma Co Ltd Method of preparing sodium hypochlorite and preparation facility for the same
US7578991B2 (en) * 2004-06-07 2009-08-25 Powell Technologies Llc Concurrent low-pressure manufacture of hypochlorite

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102009958A (en) * 2010-12-23 2011-04-13 何卫东 Device and method for producing bleacher from waste chlorine generated in lithium production
CN103241713A (en) * 2013-05-15 2013-08-14 乳源东阳光电化厂 Preparation method of sodium hypochlorite
CN103241713B (en) * 2013-05-15 2015-01-14 乳源东阳光电化厂 Preparation method of sodium hypochlorite
CN104478151A (en) * 2014-12-18 2015-04-01 重庆海洲化学品有限公司 Environment-friendly treatment method of caustic-soda-containing sodium hypochlorite waste liquor
CN104478151B (en) * 2014-12-18 2016-08-24 重庆海洲化学品有限公司 Environment-friendly treatment method containing Caustic soda sodium hypochlorite waste liquid
CN107673311A (en) * 2017-11-30 2018-02-09 山东尚舜化工有限公司 A kind of continuous device and method for preparing the high-concentrated sodium hypochlorite aqueous solution
CN111792625A (en) * 2020-08-26 2020-10-20 河北泽世康环保科技有限公司 Method for producing sodium hypochlorite
CN111792625B (en) * 2020-08-26 2023-04-28 河北泽世康环保科技有限公司 Method for producing sodium hypochlorite
CN117742278A (en) * 2024-02-07 2024-03-22 四川飞洁科技发展有限公司 Intelligent monitoring and management method and system for sodium hypochlorite production process
CN117742278B (en) * 2024-02-07 2024-04-30 四川飞洁科技发展有限公司 Intelligent monitoring and management method and system for sodium hypochlorite production process

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Application publication date: 20060719

Assignee: YIBIN HAIFENG HERUI Co.,Ltd.

Assignor: YIBIN TIANYUAN GROUP Co.,Ltd.

Contract record no.: X2022980029847

Denomination of invention: A method and device for continuous production of high-concentration sodium hypochlorite

Granted publication date: 20090121

License type: Common License

Record date: 20221230