CN106115625A - A kind of method preparing sodium hypochlorite - Google Patents
A kind of method preparing sodium hypochlorite Download PDFInfo
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- CN106115625A CN106115625A CN201610524157.3A CN201610524157A CN106115625A CN 106115625 A CN106115625 A CN 106115625A CN 201610524157 A CN201610524157 A CN 201610524157A CN 106115625 A CN106115625 A CN 106115625A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/04—Hypochlorous acid
- C01B11/06—Hypochlorites
- C01B11/062—Hypochlorites of alkali metals
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Abstract
The invention discloses a kind of method preparing sodium hypochlorite, comprise the steps: step 1: by sodium hydroxide solution dilute, and add stabilizer, stir；Step 2: sodium hydroxide solution and stabilizer after dilution enter the first cooler cooling, then are passed through film-falling absorption tower, are passed through the chlorine after cooling and react, monitor reaction end；Step 3: cool down through the second cooler, is passed through packed absorber by the product after cooling, is passed through the chlorine after cooling, monitor reaction end；Step 4: enter the 3rd cooler cooling, be passed through in finished product storage tank；Described stabilizer includes that silicon nitride, sodium silicate and sodium chloride, the addition of described silicon nitride are 3 6mg/L, and sodium silicate addition is 1 5mg/L, and the addition of sodium chloride is 1 3.5g/L.Beneficial effects of the present invention: this preparation method reduces raw material put into by improving sodium hypochlorite stability, reduces production cost and vent gas treatment cost, and the most satisfied economy is pursued but also meets the theory of environment-friendly and green.
Description
Technical field
The present invention relates to chlorine industry field, particularly to a kind of method preparing sodium hypochlorite.
Background technology
Sodium hypochlorite is a kind of high-efficient oxidant and chlorine-containing disinfectant, is used for as bleach, oxidant and water scavengine agent
Papermaking, weaving, light industry etc., have bleaching, the effect sterilizing, sterilizing.Its oxidability is strong, it is fast, effective to act on, its effect
The most extensive.In prior art, the preparation method of sodium hypochlorite mainly has saline electrolysis, chlorine and sodium hydroxide haptoreaction.
The Chinese patent of Publication No. 105197892A discloses the production technology of a kind of novel sodium hypochlorite, this production work
Artistic skill enough increases sodium hypochlorite yield, reduces operative's intensity, it is achieved stable monitoring in real time, improves monitoring accuracy.But,
This technique only increases the yield of sodium hypochlorite from the raising of speed of production, and in the production process of sodium hypochlorite, hypochlorous acid
Sodium easily decomposes, and generates sodium chloride and oxygen, thus causes available chlorine content to reduce.And in order to ensure the available chlorine content of product
Up to standard, the input of raw material can be strengthened, thus increase the cost of production cost and vent gas treatment, have much room for improvement.
Summary of the invention
It is an object of the invention to provide a kind of method preparing sodium hypochlorite.This preparation method is steady by improving sodium hypochlorite
Qualitative thus reduce raw material and put into, reduce production cost and vent gas treatment cost, not only having met economy pursues but also meets environment-friendly and green
Theory.
The above-mentioned technical purpose of the present invention has the technical scheme that
A kind of method preparing sodium hypochlorite, comprises the steps:
Step 1: by sodium hydroxide solution dilute, and add stabilizer, stir；
Step 2: the sodium hydroxide solution after dilution and stabilizer are entered the first cooler cooling, is passed through falling film absorption after cooling
Tower, and in film-falling absorption tower, be passed through the chlorine after cooling react, monitor reaction end；
Step 3: cooled down through the second cooler by the reactant liquor of step 2, is passed through packed absorber by the product after cooling, is filling out
It is passed through the chlorine after cooling in material absorption tower, monitors reaction end；
Step 4: the reactant liquor of step 3 is entered the 3rd cooler cooling, is passed through in finished product storage tank；
Described stabilizer includes that silicon nitride, sodium silicate and sodium chloride, the addition of described silicon nitride are 3-6mg/L, and sodium silicate adds
Entering amount is 1-5mg/L, and the addition of sodium chloride is 1-3.5g/L.
The present invention is further arranged to: the monitoring of reaction end relies on orp to detect device；Wherein orp detects device at one
Inert electrode detect current potential and the reacted product of film-falling absorption tower of the chlorine after the cooling being passed through film-falling absorption tower respectively
Current potential；The current potential of the chlorine after inert electrode of orp detection device detects the cooling being passed through packed absorber respectively at another
The current potential of product reacted with packed absorber.
The present invention is further arranged to: the concentration before the dilution of described sodium hydroxide is 30-35%wt.
The present invention is further arranged to: the concentration after the dilution of described sodium hydroxide is 18-22%wt.
The present invention is further arranged to: the reaction temperature controlled in film-falling absorption tower is 10-32 DEG C.
The present invention is further arranged to: control reaction temperature 10-32 DEG C in packed absorber.
The present invention is further arranged to: the effective chlorine of the product of film-falling absorption tower is at 7%-9%.
The present invention is further arranged to: the effective chlorine of the product of packed absorber is at 9%-11%.
The present invention is further arranged to: the tail gas of described film-falling absorption tower and packed absorber all enters tail gas and goes accident
Tower.
Another goal of the invention of the present invention is to provide the preparation method of a kind of stabilizer, comprises the steps:
Step1: according to weight portion, weighs 3-6 part silicon nitride, 1-5 part sodium silicate and the sodium chloride of 1000-3500 part；
Step2: the silicon nitride, sodium silicate and the sodium chloride that weighing are obtained are placed in mix homogeneously in twin-spiral mixer, are pressed into
Type；
Step3: under nitrogen protection, controls temperature 650-750 DEG C and is sintered；
Step4: the cooling laggard row of molding grinds, crosses 200 mesh sieves and obtains product.
In sum, the method have the advantages that
1, the present invention adds stabilizer in the preparation process of sodium hypochlorite, strengthens the stability of sodium hypochlorite, so that having
Effect chlorine required raw material up to standard reduces, and reduces production cost and vent gas treatment cost；
2, silicon nitride is white powder crystal, and heat stability is high, oxidation resistance strong, has an effect hardly with water, dense by force
In acid solution, slowly hydrolysis generates ammonium salt and silicon dioxide.Sodium silicate is soluble in water, and its aqueous solution is long placed in atmosphere can be because inhaling
Receive carbon dioxide and produce silicic acid precipitation.Sodium chloride is soluble in water, ionizes out chloride ion in water such that it is able to suppression hypochlorous acid
Sodium decomposes.Can interact between silicon nitride and sodium silicate inventors have surprisingly discovered that, mutually promote, common enhancing time chlorine
The stability of acid sodium；
3, silicon nitride, sodium silicate and sodium chloride being sintered, strengthen silicon nitride, sodium silicate and the effect of sodium chloride, it is right to promote
The stability of sodium hypochlorite；
4, utilize orp to carry out on-line real time monitoring reaction process, it is not necessary to arrangement personnel analyze in real time, reduce employee work strong
Degree, improves production efficiency.
Accompanying drawing explanation
Fig. 1 is the preparation technology figure of sodium hypochlorite.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail.
This specific embodiment is only explanation of the invention, and it is not limitation of the present invention, people in the art
The present embodiment can be made after reading this specification by member as required does not has the amendment of creative contribution, but as long as at this
All protected by Patent Law in the right of invention.
Embodiment 1-5 is the preparation embodiment of stabilizer.
Embodiment 1
Step1: according to weight portion, weighs 3 parts of silicon nitrides, 4 parts of sodium silicate and the sodium chloride of 1000 parts；
Step2: the silicon nitride, sodium silicate and the sodium chloride that weighing are obtained are placed in mix homogeneously in twin-spiral mixer, are pressed into
Type；
Step3: under nitrogen protection, controls temperature 650 DEG C and is sintered；
Step4: the cooling laggard row of molding grinds, crosses 200 mesh sieves and obtains product.
Embodiment 2
Step1: according to weight portion, weighs 4 parts of silicon nitrides, 2 parts of sodium silicate and the sodium chloride of 1500 parts；
Step2: the silicon nitride, sodium silicate and the sodium chloride that weighing are obtained are placed in mix homogeneously in twin-spiral mixer, are pressed into
Type；
Step3: under nitrogen protection, controls temperature 675 DEG C and is sintered；
Step4: the cooling laggard row of molding grinds, crosses 200 mesh sieves and obtains product.
Embodiment 3
Step1: according to weight portion, weighs 6 parts of silicon nitrides, 3 parts of sodium silicate and the sodium chloride of 2000 parts；
Step2: the silicon nitride, sodium silicate and the sodium chloride that weighing are obtained are placed in mix homogeneously in twin-spiral mixer, are pressed into
Type；
Step3: under nitrogen protection, controls temperature 700 DEG C and is sintered；
Step4: the cooling laggard row of molding grinds, crosses 200 mesh sieves and obtains product.
Embodiment 4
Step1: according to weight portion, weighs 3 parts of silicon nitrides, 5 parts of sodium silicate and the sodium chloride of 2500 parts；
Step2: the silicon nitride, sodium silicate and the sodium chloride that weighing are obtained are placed in mix homogeneously in twin-spiral mixer, are pressed into
Type；
Step3: under nitrogen protection, controls temperature 725 DEG C and is sintered；
Step4: the cooling laggard row of molding grinds, crosses 200 mesh sieves and obtains product.
Embodiment 5
Step1: according to weight portion, weighs 4 parts of silicon nitrides, 2 parts of sodium silicate and the sodium chloride of 3500 parts；
Step2: the silicon nitride, sodium silicate and the sodium chloride that weighing are obtained are placed in mix homogeneously in twin-spiral mixer, are pressed into
Type；
Step3: under nitrogen protection, controls temperature 750 DEG C and is sintered；
Step4: the cooling laggard row of molding grinds, crosses 200 mesh sieves and obtains product.
With reference to Fig. 1, embodiment 6-10 is the preparation method embodiment of sodium hypochlorite.
The monitoring of the reaction end in embodiment 6-10 relies on orp to detect device, orp detection device include inert electrode with
And reference electrode.Chlorine after wherein the inert electrode of orp detection device detects the cooling being passed through film-falling absorption tower respectively at one
Current potential and the current potential of the reacted product of film-falling absorption tower.At another, the inert electrode of orp detection device detects respectively and is passed through
The current potential of the chlorine after the cooling of packed absorber and the current potential of the reacted product of packed absorber.
Embodiment 6
Stabilizer uses the stabilizer according to embodiment 1 preparation.
Step 1: the sodium hydroxide solution of 30%wt is diluted with water to 18%wt, and adds according to 1.007g/L stable
Agent, stirs；
Step 2: the sodium hydroxide solution after dilution and stabilizer are entered the first cooler cooling, is passed through falling film absorption after cooling
Tower, and in film-falling absorption tower, be passed through the chlorine after cooling react, controlling reaction temperature is 10 DEG C, monitors reaction end,
Tail gas enters tail gas and removes accident tower；
Step 3: cooled down through the second cooler by the reactant liquor of step 2, is passed through packed absorber by the product after cooling, is filling out
Being passed through the chlorine after cooling in material absorption tower, controlling reaction temperature is 10 DEG C, monitors reaction end, and tail gas enters tail gas and goes accident
Tower；Step 4: the reactant liquor of step 3 is entered the 3rd cooler cooling, is passed through in finished product storage tank.
Embodiment 7
Stabilizer uses the stabilizer according to embodiment 2 preparation.
Step 1: the sodium hydroxide solution of 31%wt is diluted with water to 19%wt, and adds according to 1.506g/L stable
Agent, stirs；
Step 2: the sodium hydroxide solution after dilution and stabilizer are entered the first cooler cooling, is passed through falling film absorption after cooling
Tower, and in film-falling absorption tower, be passed through the chlorine after cooling react, controlling reaction temperature is 15 DEG C, monitors reaction end,
Tail gas enters tail gas and removes accident tower；
Step 3: cooled down through the second cooler by the reactant liquor of step 2, is passed through packed absorber by the product after cooling, is filling out
Being passed through the chlorine after cooling in material absorption tower, controlling reaction temperature is 15 DEG C, monitors reaction end, and tail gas enters tail gas and goes accident
Tower；Step 4: the reactant liquor of step 3 is entered the 3rd cooler cooling, is passed through in finished product storage tank.
Embodiment 8
Stabilizer uses the stabilizer according to embodiment 3 preparation.
Step 1: the sodium hydroxide solution of 32%wt is diluted with water to 20%wt, and adds according to 2.008g/L stable
Agent, stirs；
Step 2: the sodium hydroxide solution after dilution and stabilizer are entered the first cooler cooling, is passed through falling film absorption after cooling
Tower, and in film-falling absorption tower, be passed through the chlorine after cooling react, controlling reaction temperature is 20 DEG C, monitors reaction end,
Tail gas enters tail gas and removes accident tower；
Step 3: cooled down through the second cooler by the reactant liquor of step 2, is passed through packed absorber by the product after cooling, is filling out
Being passed through the chlorine after cooling in material absorption tower, controlling reaction temperature is 20 DEG C, monitors reaction end, and tail gas enters tail gas and goes accident
Tower；Step 4: the reactant liquor of step 3 is entered the 3rd cooler cooling, is passed through in finished product storage tank.
Embodiment 9
Stabilizer uses the stabilizer according to embodiment 4 preparation.
Step 1: the sodium hydroxide solution of 33%wt is diluted with water to 21%wt, and adds according to 2.507g/L stable
Agent, stirs；
Step 2: the sodium hydroxide solution after dilution and stabilizer are entered the first cooler cooling, is passed through falling film absorption after cooling
Tower, and in film-falling absorption tower, be passed through the chlorine after cooling react, controlling reaction temperature is 25 DEG C, monitors reaction end,
Tail gas enters tail gas and removes accident tower；
Step 3: cooled down through the second cooler by the reactant liquor of step 2, is passed through packed absorber by the product after cooling, is filling out
Being passed through the chlorine after cooling in material absorption tower, controlling reaction temperature is 25 DEG C, monitors reaction end, and tail gas enters tail gas and goes accident
Tower；Step 4: the reactant liquor of step 3 is entered the 3rd cooler cooling, is passed through in finished product storage tank.
Embodiment 10
Stabilizer uses the stabilizer according to embodiment 5 preparation.
Step 1: the sodium hydroxide solution of 35%wt is diluted with water to 22%wt, and adds according to 3.006g/L stable
Agent, stirs；
Step 2: the sodium hydroxide solution after dilution and stabilizer are entered the first cooler cooling, is passed through falling film absorption after cooling
Tower, and in film-falling absorption tower, be passed through the chlorine after cooling react, controlling reaction temperature is 32 DEG C, monitors reaction end,
Tail gas enters tail gas and removes accident tower；
Step 3: cooled down through the second cooler by the reactant liquor of step 2, is passed through packed absorber by the product after cooling, is filling out
Being passed through the chlorine after cooling in material absorption tower, controlling reaction temperature is 32 DEG C, monitors reaction end, and tail gas enters tail gas and goes accident
Tower；Step 4: the reactant liquor of step 3 is entered the 3rd cooler cooling, is passed through in finished product storage tank.
Comparative example 1
Select the embodiment 1 as a comparison case 1 of the Chinese patent of publication number 105197892A.
Comparative example 2
The sodium silicate that silicon nitride in stabilizer use etc. weigh as different from Example 5 substitutes, and other is same as in Example 5.
Comparative example 3
The silicon nitride that sodium silicate in stabilizer use etc. weigh as different from Example 5 substitutes, and other is same as in Example 5.
The 20%wt sodium hydroxide concentration of embodiment 6-10 and comparative example 1-3 is 10L, and flow velocity is 1.2m/s, chlorine according to
Quality of chlorine gas is 1: 2.5 use with the mass ratio of sodium hydroxide, and chlorine flow velocity is 8m/s.In film-falling absorption tower, chlorine usage amount is
70% (volume) of the total consumption of chlorine, remains in packed absorber and uses.Measure embodiment 6-10 and comparative example 1-3 falling liquid film is inhaled
Receive the available chlorine content of the product of tower and packed absorber.
The available chlorine content record of the product of table 1 embodiment 6-10 and comparative example 1-3 film-falling absorption tower and packed absorber
Table
It is concluded that from table 1
Comparative example 6-10 understands with comparative example 1, under the conditions of the sodium hydroxide and chlorine of equivalent, and the falling liquid film of embodiment 6-10
The available chlorine content on absorption tower and the available chlorine content of packed absorber are above comparative example 1.Visible, when needs produce up to target
During sodium hypochlorite, use the present invention provide sodium hypochlorite preparation method needed for raw material less, reduce production cost and
Vent gas treatment cost.
Comparative example 6-10 and comparative example 2-3 understand, under the conditions of the sodium hydroxide and chlorine of equivalent, and embodiment 6-10
The available chlorine content of film-falling absorption tower and the available chlorine content of packed absorber be above comparative example 2 and 3, and comparative example 2
The available chlorine content of film-falling absorption tower and the available chlorine content of packed absorber be above comparative example 3.Visible, silicon nitride and silicon
Cooperative effect can be produced between acid sodium, improve the stability of sodium hypochlorite.
Claims (10)
1. the method preparing sodium hypochlorite, is characterized in that: comprise the steps:
Step 1: by sodium hydroxide solution dilute, and add stabilizer, stir；
Step 2: the sodium hydroxide solution after dilution and stabilizer are entered the first cooler cooling, is passed through falling film absorption after cooling
Tower, and in film-falling absorption tower, be passed through the chlorine after cooling react, monitor reaction end；
Step 3: cooled down through the second cooler by the reactant liquor of step 2, is passed through packed absorber by the product after cooling, is filling out
It is passed through the chlorine after cooling in material absorption tower, monitors reaction end；
Step 4: the reactant liquor of step 3 is entered the 3rd cooler cooling, is passed through in finished product storage tank；
Described stabilizer includes that silicon nitride, sodium silicate and sodium chloride, the addition of described silicon nitride are 3-6mg/L, and sodium silicate adds
Entering amount is 1-5mg/L, and the addition of sodium chloride is 1-3.5g/L.
A kind of method preparing sodium hypochlorite the most according to claim 1, is characterized in that: the monitoring of reaction end relies on
Orp detects device；Chlorine after wherein the inert electrode of orp detection device detects the cooling being passed through film-falling absorption tower respectively at one
Current potential and the current potential of the reacted product of film-falling absorption tower；At another, the inert electrode of orp detection device detects respectively and is passed through
The current potential of the chlorine after the cooling of packed absorber and the current potential of the reacted product of packed absorber.
A kind of method preparing sodium hypochlorite the most according to claim 1, is characterized in that: before the dilution of described sodium hydroxide
Concentration is 30-35%wt.
A kind of method preparing sodium hypochlorite the most according to claim 1, is characterized in that: after the dilution of described sodium hydroxide
Concentration is 18-22%wt.
A kind of method preparing sodium hypochlorite the most according to claim 1, is characterized in that: control in film-falling absorption tower is anti-
Temperature is answered to be 10-32 DEG C.
A kind of method preparing sodium hypochlorite the most according to claim 1, is characterized in that: control in packed absorber is anti-
Answer temperature 10-32 DEG C.
A kind of method preparing sodium hypochlorite the most according to claim 1, is characterized in that: the product of film-falling absorption tower
Effective chlorine at 7%-9%.
A kind of method preparing sodium hypochlorite the most according to claim 1, is characterized in that: the product of packed absorber
Effective chlorine at 9%-11%.
A kind of method preparing sodium hypochlorite the most according to claim 1, is characterized in that: described film-falling absorption tower and filler
The tail gas on absorption tower all enters tail gas and removes accident tower.
10. a preparation method for stabilizer as claimed in claim 1, is characterized in that: comprise the steps:
Step1: according to weight portion, weighs 3-6 part silicon nitride, 1-5 part sodium silicate and the sodium chloride of 1000-3500 part；
Step2: the silicon nitride, sodium silicate and the sodium chloride that weighing are obtained are placed in mix homogeneously in twin-spiral mixer, are pressed into
Type；
Step3: under nitrogen protection, controls temperature 650-750 DEG C and is sintered；
Step4: the cooling laggard row of molding grinds, crosses 200 mesh sieves and obtains product.
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Cited By (2)
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| CN110367275A (en) * | 2019-06-19 | 2019-10-25 | 山东消博士消毒科技股份有限公司 | A kind of thimerosal and preparation method thereof |
| CN110817806A (en) * | 2019-12-12 | 2020-02-21 | 宁夏华御化工有限公司 | High-concentration sodium hypochlorite co-production device and method |
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Address after: 315204 No. 655 Haitian Road, Ningbo Petrochemical Economic Development Zone, Zhenhai District, Zhejiang, Ningbo, China Patentee after: Zhejiang Zhenyang Development Co., Ltd Address before: 315204 Chemical Industrial Zone, Zhejiang, Ningbo, China Patentee before: NINGBO OCEANKING CHEMICAL DEVELOPMENT Co.,Ltd. |