CN106698744A - Method for removing hydrazine hydrate in H acid waste water - Google Patents
Method for removing hydrazine hydrate in H acid waste water Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1493—Selection of liquid materials for use as absorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/30—Alkali metal compounds
- B01D2251/304—Alkali metal compounds of sodium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2251/604—Hydroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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Abstract
The invention relates to a method for removing hydrazine hydrate in H acid waste water. The method comprises the following steps: denitration, primary reduction, secondary reduction and T acid segregation. The method is scientific and reasonable, further reduces water solution and protects the environment.
Description
Technical field
The present invention relates to the side of hydrazine hydrate in hydrazine hydrate, more particularly to a kind of removal H acid waste water in one kind removal H acid waste water
Method.
Background technology
H acid commodity are usually paste or powder.Cold water is slightly soluble in, is dissolved in the alkaline solutions such as soda ash and caustic soda.H- acid
Mono-sodium salt mainly for the production of acidity, directly and reactive dye, such as acid fuchsin 6b, acid red G, Acid Black 10B, directly
Black, Reactive Brilliant Red K-2BP, active purple k-3r, molten blue K-R of activity etc. more than 90 is planted, and these dyestuffs are used for wool spinning, the dye of bafta
Color.
It is domestic main at present using " three sulfonation-alkali fusion " production H acid, will naphthalene sulfuric acid or 65% oleum enter
Row sulfonation, obtains 1,3,6- naphthalene trisulfonic acids, then through in mixed acid nitrification, ammoniacal liquor and reduction obtains T acid ammonium salts, then by alkali fusion
H acid is obtained with acidifying.Prepared by traditional T acid is to use iron powder reducing technique, although iron powder reducing technique cost is very low, is produced big
Amount solid waste, so being eliminated already.The substitute is hydrogenating reduction and hydrazine hydrate reduction technique.Because using hydrazine hydrate reduction work
Little is changed to original equipment when skill replaces iron powder technique, so using commonplace.But during hydrazine hydrate reduction, in order that 8- nitre
Base -1,3,6- trisulfonic acid ammonium salts conversion often makes hydrazine hydrate excessive more than 25% completely, and this large amount of hydrazine hydrate is not only unrestrained
Expense is fallen, but also serious pollution is caused to environment.
The content of the invention
The present invention mainly solves the deficiencies in the prior art, there is provided one kind is with insufficient amount of hydrazine hydrate to 8- nitre
Base -1,3,6- trisulfonic acid ammonium salts are reduced, after ruing out of hydrazine hydrate, then with another reducing agent by remaining 8- nitros -
The reduction of 1,3,6- trisulfonic acid ammonium salt is complete, and a kind of removal H acid waste water of the pollution problem of hydrazine hydrate is so solved from source
The method of middle hydrazine hydrate.
Above-mentioned technical problem of the invention is mainly what is be addressed by following technical proposals：
The method of hydrazine hydrate, is carried out according to the following steps in a kind of removal H acid waste water：
A. denitration：With 3~4 hours to being passed through 4700 part 4% of aqueous sodium carbonate from bottom in 3500 parts of nitrification materials,
Tail gas concentration is 32% sodium hydrate aqueous solution absorption；Whether sampling detection sees arrive terminal；If less than terminal, it is necessary to again
Add 300~500 part 4% of aqueous sodium carbonate；
B. once reduce：It is that 20% ammoniacal liquor adjustment pH value is 8~9 with concentration, adds 25 parts of catalyst, is warming up to 95 DEG C,
With 4 hours to being added dropwise the hydrazine hydrate that 200 parts of concentration are 80% in substrate, concentration be 80% hydrazine hydrate equivalent to 8- nitro -1,
1.4 times of 3,6- trisulfonic acid naphthalene molal quantitys, then run out of in 95~100 DEG C of reaction to hydrazine hydrates；
C. secondary reduction：It is 3 to adjust pH value with a small amount of hydrochloric acid, keeps temperature of charge at 95~100 DEG C；It is slowly added to 50 parts
Reducing agent, continues to be incubated 3 hours at 100~104 DEG C, is controlled in sampling；If not being reacted to terminal, continue at 100~104 DEG C
Insulation is complete to reaction；Catalyst is filtered out, recovery is used for multiple times, manufacturer's regeneration is returned after failure, mother liquor is collected；
D.T acid isolations：It is 1~2 to adjust mother liquor pH value with sulfuric acid, is subsequently adding 800 parts of anhydrous sodium sulfates；Continue to be cooled to 40
DEG C, T acid is filtered to obtain in stirring after 2 hours；
Preferably, described catalyst is Raney's nickel or Fe (OH)3/C；Wherein the addition of Raney's nickel be 8- nitros-
The 1~10% of 1,3,6- trisulfonic acid naphthalene, Raney's nickel can be reused.
Preferably, described catalyst selects Fe (OH)3During/C, the method matched somebody with somebody is：By 30 parts of Iron(III) chloride hexahydrates
In adding 300 parts of water with 5 points of activated carbons, be heated to 60~70 DEG C and stir 0.5 hour, then added under stirring 8- nitros-
In the ammonium salt material of 1,3,6- trisulfonic acid naphthalene；Addition is 8- nitro -1, the 1~10% of 3,6- trisulfonic acid naphthalenes.
Preferably, described hydrazine hydrate and 8- nitro -1, the mol ratio of 3,6- trisulfonic acid naphthalenes is (1.0 ︰ 1)~(1.5 ︰
1)。
Preferably, the used reducing agent of described second reduction be iron powder, zinc powder, vulcanized sodium, NaHS and
Sodium polysulfide one kind therein.
Preferably, described judgement 8- nitro -1,3,6- trisulfonic acid naphthalene ammonium salts are fully converted to 8- amino -1,3,6- tri-
The method of sulfonic acid naphthalene ammonium salt is：The material for having reduced is taken, constant volume surveys amino value and is designated as A1, same material is added substantial amounts of
Zinc powder, is warming up to boiling, and it is 3 to adjust pH value with hydrochloric acid, is kept for 10 minutes, is then filtered, constant volume, measures amino value and is designated as A2, (A2﹣
A1)÷A1When × 100%≤0.5, for reaction is complete.
The method is scientific and reasonable, further reduces water pollution, environmental protection.
Specific embodiment
Below by embodiment, technical scheme is described in further detail.
Embodiment 1：The method of hydrazine hydrate, is carried out according to the following steps in a kind of removal H acid waste water：
A. denitration：With 3 hours to being passed through 4700 part 4% of aqueous sodium carbonate, tail from bottom in 3500 parts of nitrification materials
Gas concentration is 32% sodium hydrate aqueous solution absorption；Whether sampling detection sees arrive terminal；If less than terminal, it is necessary to add again
Enter 300 part 4% of aqueous sodium carbonate；
B. once reduce：It is that 20% ammoniacal liquor adjustment pH value is 8 with concentration, adds 25 parts of catalyst, 95 DEG C is warming up to, with 4
Hour to being added dropwise the hydrazine hydrate that 200 parts of concentration are 80% in substrate, concentration be 80% hydrazine hydrate equivalent to 8- nitro -1,3,6-
1.4 times of trisulfonic acid naphthalene molal quantity, then run out of in 95 DEG C of reaction to hydrazine hydrates；
C. secondary reduction：It is 3 to adjust pH value with a small amount of hydrochloric acid, keeps temperature of charge at 95 DEG C；It is slowly added to 50 parts of reduction
Agent, continues to be incubated 3 hours at 100 DEG C, is controlled in sampling；If not being reacted to terminal, continue in 100 DEG C of insulations to having reacted
Entirely；Catalyst is filtered out, recovery is used for multiple times, manufacturer's regeneration is returned after failure, mother liquor is collected；
D.T acid isolations：It is 1 to adjust mother liquor pH value with sulfuric acid, is subsequently adding 800 parts of anhydrous sodium sulfates；Continue to be cooled to 40 DEG C,
T acid is filtered to obtain in stirring after 2 hours；
Described catalyst is Raney's nickel；Wherein the addition of Raney's nickel be 8- nitro -1,3,6- trisulfonic acid naphthalenes 1~
10%, Raney's nickel can be reused.
Described hydrazine hydrate and 8- nitro -1, the mol ratio of 3,6- trisulfonic acid naphthalenes is (1.0 ︰ 1)~(1.5 ︰ 1).
The used reducing agent of described second reduction for iron powder, zinc powder, vulcanized sodium, NaHS and sodium polysulfide its
In one kind.
Described judgement 8- nitro -1,3,6- trisulfonic acid naphthalene ammonium salts are fully converted to 8- amino -1,3,6- trisulfonic acid naphthalene ammoniums
The method of salt is：The material for having reduced is taken, constant volume surveys amino value and is designated as A1, same material is added into substantial amounts of zinc powder, heat up
To seething with excitement, it is 3 to adjust pH value with hydrochloric acid, is kept for 10 minutes, is then filtered, constant volume, measures amino value and is designated as A2, (A2﹣ A1)÷A1×
When 100%≤0.5, for reaction is complete.
Embodiment 2：The method of hydrazine hydrate, is carried out according to the following steps in a kind of removal H acid waste water：
A. denitration：With 3.5 hours to being passed through 4700 part 4% of aqueous sodium carbonate from bottom in 3500 parts of nitrification materials,
Tail gas concentration is 32% sodium hydrate aqueous solution absorption；Whether sampling detection sees arrive terminal；If less than terminal, it is necessary to again
Add 400 part 4% of aqueous sodium carbonate；
B. once reduce：It is that 20% ammoniacal liquor adjustment pH value is 8.5 with concentration, adds 25 parts of catalyst, be warming up to 95 DEG C, uses
4 hours to being added dropwise the hydrazine hydrate that 200 parts of concentration are 80% in substrate, concentration be 80% hydrazine hydrate equivalent to 8- nitro -1,3,
1.4 times of 6- trisulfonic acid naphthalene molal quantitys, then run out of in 98 DEG C of reaction to hydrazine hydrates；
C. secondary reduction：It is 3 to adjust pH value with a small amount of hydrochloric acid, keeps temperature of charge at 98 DEG C；It is slowly added to 50 parts of reduction
Agent, continues to be incubated 3 hours at 101 DEG C, is controlled in sampling；If not being reacted to terminal, continue in 101 DEG C of insulations to having reacted
Entirely；Catalyst is filtered out, recovery is used for multiple times, manufacturer's regeneration is returned after failure, mother liquor is collected；
D.T acid isolations：It is 1.5 to adjust mother liquor pH value with sulfuric acid, is subsequently adding 800 parts of anhydrous sodium sulfates；Continue to be cooled to 40
DEG C, T acid is filtered to obtain in stirring after 2 hours；
Described catalyst is Fe (OH)3/C。
Described catalyst selects Fe (OH)3During/C, the method matched somebody with somebody is：By 30 parts of Iron(III) chloride hexahydrates and 5 points of activity
Charcoal is added in 300 parts of water, is heated to 60~70 DEG C and is stirred 0.5 hour, and 8- nitro -1,3,6- tri- sulphurs are then added under stirring
In the ammonium salt material of sour naphthalene；Addition is 8- nitro -1, the 1~10% of 3,6- trisulfonic acid naphthalenes.
Described hydrazine hydrate and 8- nitro -1, the mol ratio of 3,6- trisulfonic acid naphthalenes is (1.0 ︰ 1)~(1.5 ︰ 1).
The used reducing agent of described second reduction for iron powder, zinc powder, vulcanized sodium, NaHS and sodium polysulfide its
In one kind.
Described judgement 8- nitro -1,3,6- trisulfonic acid naphthalene ammonium salts are fully converted to 8- amino -1,3,6- trisulfonic acid naphthalene ammoniums
The method of salt is：The material for having reduced is taken, constant volume surveys amino value and is designated as A1, same material is added into substantial amounts of zinc powder, heat up
To seething with excitement, it is 3 to adjust pH value with hydrochloric acid, is kept for 10 minutes, is then filtered, constant volume, measures amino value and is designated as A2, (A2﹣ A1)÷A1×
When 100%≤0.5, for reaction is complete.
Embodiment 3：The method of hydrazine hydrate, is carried out according to the following steps in a kind of removal H acid waste water：
A. denitration：With 4 hours to being passed through 4700 part 4% of aqueous sodium carbonate, tail from bottom in 3500 parts of nitrification materials
Gas concentration is 32% sodium hydrate aqueous solution absorption；Whether sampling detection sees arrive terminal；If less than terminal, it is necessary to add again
Enter 500 part 4% of aqueous sodium carbonate；
B. once reduce：It is that 20% ammoniacal liquor adjustment pH value is 9 with concentration, adds 25 parts of catalyst, 95 DEG C is warming up to, with 4
Hour to being added dropwise the hydrazine hydrate that 200 parts of concentration are 80% in substrate, concentration be 80% hydrazine hydrate equivalent to 8- nitro -1,3,6-
1.4 times of trisulfonic acid naphthalene molal quantity, then run out of in 100 DEG C of reaction to hydrazine hydrates；
C. secondary reduction：It is 3 to adjust pH value with a small amount of hydrochloric acid, keeps temperature of charge at 100 DEG C；It is slowly added to 50 parts of reduction
Agent, continues to be incubated 3 hours at 104 DEG C, is controlled in sampling；If not being reacted to terminal, continue in 104 DEG C of insulations to having reacted
Entirely；Catalyst is filtered out, recovery is used for multiple times, manufacturer's regeneration is returned after failure, mother liquor is collected；
D.T acid isolations：It is 2 to adjust mother liquor pH value with sulfuric acid, is subsequently adding 800 parts of anhydrous sodium sulfates；Continue to be cooled to 40 DEG C,
T acid is filtered to obtain in stirring after 2 hours；
Described catalyst is Raney's nickel.
Described hydrazine hydrate and 8- nitro -1, the mol ratio of 3,6- trisulfonic acid naphthalenes is (1.0 ︰ 1)~(1.5 ︰ 1).
The used reducing agent of described second reduction for iron powder, zinc powder, vulcanized sodium, NaHS and sodium polysulfide its
In one kind.
Described judgement 8- nitro -1,3,6- trisulfonic acid naphthalene ammonium salts are fully converted to 8- amino -1,3,6- trisulfonic acid naphthalene ammoniums
The method of salt is：The material for having reduced is taken, constant volume surveys amino value and is designated as A1, same material is added into substantial amounts of zinc powder, heat up
To seething with excitement, it is 3 to adjust pH value with hydrochloric acid, is kept for 10 minutes, is then filtered, constant volume, measures amino value and is designated as A2, (A2﹣ A1)÷A1×
When 100%≤0.5, for reaction is complete.
Claims (6)
1. in a kind of removal H acid waste water hydrazine hydrate method, it is characterised in that carry out according to the following steps：
A. denitration：With 3~4 hours to being passed through 4700 part 4% of aqueous sodium carbonate, tail gas from bottom in 3500 parts of nitrification materials
Absorbed with the sodium hydrate aqueous solution that concentration is 32%；Whether sampling detection sees arrive terminal；If less than terminal, it is necessary to add
300~500 part 4% of aqueous sodium carbonate；
B. once reduce：It is that to adjust pH value be 8~9 to 20% ammoniacal liquor with concentration, adds 25 parts of catalyst, is warming up to 95 DEG C, it is small with 4
When to being added dropwise the hydrazine hydrate that 200 parts of concentration are 80% in substrate, concentration be 80% hydrazine hydrate equivalent to 8- nitro -1,3,6- tri-
1.4 times of sulfonic acid naphthalene molal quantity, then run out of in 95~100 DEG C of reaction to hydrazine hydrates；
C. secondary reduction：It is 3 to adjust pH value with a small amount of hydrochloric acid, keeps temperature of charge at 95~100 DEG C；It is slowly added to 50 parts of reduction
Agent, continues to be incubated 3 hours at 100~104 DEG C, is controlled in sampling；If not being reacted to terminal, continue in 100~104 DEG C of insulations
It is complete to reacting；Catalyst is filtered out, recovery is used for multiple times, manufacturer's regeneration is returned after failure, mother liquor is collected；
D.T acid isolations：It is 1~2 to adjust mother liquor pH value with sulfuric acid, is subsequently adding 800 parts of anhydrous sodium sulfates；Continue to be cooled to 40 DEG C,
T acid is filtered to obtain in stirring after 2 hours.
2. in a kind of removal H acid waste water according to claim 1 hydrazine hydrate method, it is characterised in that：Described catalysis
Agent is Raney's nickel or Fe (OH)3/C；Wherein the addition of Raney's nickel is 8- nitro -1, the 1~10% of 3,6- trisulfonic acid naphthalenes, thunder Buddhist nun
Nickel can be reused.
3. in a kind of removal H acid waste water according to claim 2 hydrazine hydrate method, it is characterised in that：Described catalysis
Fe (OH) is selected in agent3During/C, the method matched somebody with somebody is：During 30 parts of Iron(III) chloride hexahydrates and 5 points of activated carbons are added into 300 parts of water, plus
Hot to 60~70 DEG C are stirred 0.5 hour, 8- nitro -1 are then added under stirring, in the ammonium salt material of 3,6- trisulfonic acid naphthalenes；
Addition is 8- nitro -1, the 1~10% of 3,6- trisulfonic acid naphthalenes.
4. in a kind of removal H acid waste water according to claim 1 hydrazine hydrate method, it is characterised in that：Described hydration
Hydrazine and 8- nitro -1, the mol ratio of 3,6- trisulfonic acid naphthalenes is (1.0 ︰ 1)~(1.5 ︰ 1).
5. in a kind of removal H acid waste water according to claim 1 hydrazine hydrate method, it is characterised in that：Described second
The used reducing agent of secondary reduction is iron powder, zinc powder, vulcanized sodium, NaHS and sodium polysulfide one kind therein.
6. in a kind of removal H acid waste water according to claim 1 hydrazine hydrate method, it is characterised in that：Described judgement
8- nitro -1,3,6- trisulfonic acid naphthalene ammonium salts are fully converted to 8- amino -1, and the method for 3,6- trisulfonic acid naphthalene ammonium salts is：Take and reduce
Material, constant volume, survey amino value be designated as A1, same material is added into substantial amounts of zinc powder, boiling is warming up to, adjust pH value with hydrochloric acid
It is 3, is kept for 10 minutes, then filter, constant volume, measures amino value and be designated as A2, (A2﹣ A1)÷A1It is reaction when × 100%≤0.5
Completely.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107602422A (en) * | 2017-09-11 | 2018-01-19 | 吴江梅堰三友染料化工有限公司 | A kind of clean type product 1,6,1,7 mixes the preparation method of 1-naphthlamine-6-sulfonic acid |
| CN114230078A (en) * | 2021-12-21 | 2022-03-25 | 武汉瑞阳化工有限公司 | Comprehensive utilization method of acidic wastewater generated in 1-fluoronaphthalene production |
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| CN107602422A (en) * | 2017-09-11 | 2018-01-19 | 吴江梅堰三友染料化工有限公司 | A kind of clean type product 1,6,1,7 mixes the preparation method of 1-naphthlamine-6-sulfonic acid |
| CN107602422B (en) * | 2017-09-11 | 2020-05-29 | 吴江梅堰三友染料化工有限公司 | Preparation method of cleaning type product 1,6, 1,7 mixed clevuric acid |
| CN114230078A (en) * | 2021-12-21 | 2022-03-25 | 武汉瑞阳化工有限公司 | Comprehensive utilization method of acidic wastewater generated in 1-fluoronaphthalene production |
| CN114230078B (en) * | 2021-12-21 | 2023-09-22 | 武汉瑞阳化工有限公司 | Comprehensive utilization method of acid wastewater generated in production of 1-fluoronaphthalene |
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