CN101712485B - Preparation method of basic zinc chloride - Google Patents
Preparation method of basic zinc chloride Download PDFInfo
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- CN101712485B CN101712485B CN2009103104209A CN200910310420A CN101712485B CN 101712485 B CN101712485 B CN 101712485B CN 2009103104209 A CN2009103104209 A CN 2009103104209A CN 200910310420 A CN200910310420 A CN 200910310420A CN 101712485 B CN101712485 B CN 101712485B
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- CN
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- Prior art keywords
- zinc chloride
- basic zinc
- preparation
- reaction
- zinc
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- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 title claims abstract description 71
- 235000005074 zinc chloride Nutrition 0.000 title claims abstract description 36
- 239000011592 zinc chloride Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 24
- 239000000047 product Substances 0.000 abstract description 21
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000001035 drying Methods 0.000 abstract description 6
- 239000002699 waste material Substances 0.000 abstract description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 2
- 239000011701 zinc Substances 0.000 description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 14
- 229910052725 zinc Inorganic materials 0.000 description 14
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
- 229910052785 arsenic Inorganic materials 0.000 description 5
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 5
- 229910052793 cadmium Inorganic materials 0.000 description 5
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 241001465754 Metazoa Species 0.000 description 3
- 239000002826 coolant Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003053 immunization Effects 0.000 description 2
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 2
- 229960001763 zinc sulfate Drugs 0.000 description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 description 2
- 206010012735 Diarrhoea Diseases 0.000 description 1
- 241000282887 Suidae Species 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 230000002180 anti-stress Effects 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 210000003746 feather Anatomy 0.000 description 1
- 230000003031 feeding effect Effects 0.000 description 1
- 230000004720 fertilization Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000037308 hair color Effects 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 235000019629 palatability Nutrition 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 230000003245 working effect Effects 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- -1 zinc oxide Chemical class 0.000 description 1
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- Fodder In General (AREA)
Abstract
The invention discloses a preparation method of basic zinc chloride, comprising the following steps of: adding sodium hydroxide or ammonia water into zinc chloride solution with the mol ratio of the sodium hydroxide or ammonia water to zinc chloride solution of 7.5-8.5:5, reacting under the condition that the temperature is 60-105 DEG C and the pH value is 5-9, and obtaining reaction products after the reaction is finished; and washing with water, centrifuging and drying reaction products to obtain the basic zinc chloride. The preparation method is simple and safe in operation, and has the advantages of little waste emission, low production cost and excellent product quality.
Description
Technical field
The present invention relates to a kind of preparation method of compound of zinc, relate in particular to a kind of halid preparation method of zinc.
Background technology
Basic zinc chloride is as a kind of new zinc source feed additive; With respect to conventional zinc sources such as zinc oxide and zinc sulfate; Have that the interpolation level is low, consumption is few, advantage such as good palatability, biological value height and feeding effect are good; And more help protecting environment, be a kind of safe, efficient, environmental protection and comprehensive effects novel fodder additive.In the process for producing of present existing basic zinc chloride, useful useless zinc is produced, useful zinc chloride and zinc oxide reacted; Also useful hydrochloric acid and zinc oxide or react with hydrochloric acid and zinc subcarbonate and to produce; In these preparing methods, the method production cost that has is too high, and the raw materials used price of the method that has is relatively costly; The preparing method's gained by product that has causes environmental pollution easily, all has certain limitation.
Summary of the invention
The technical problem that the present invention will solve is the deficiency that overcomes prior art, and a kind of safety simple to operate, waste discharge is few, production cost is low and the product quality is better preparation method of basic zinc chloride are provided.
For solving the problems of the technologies described above; The technical scheme that the present invention proposes is a kind of preparation method of basic zinc chloride; May further comprise the steps: sodium hydroxide or ammoniacal liquor are added in the liquor zinci chloridi; The mol ratio of said sodium hydroxide or ammoniacal liquor and zinc chloride is (7.5～8.5): 5, and be that 60 ℃～105 ℃, pH value are to react under 5～9 the condition in temperature, reaction obtains reaction product after accomplishing; With making basic zinc chloride after reaction product washing, centrifugal, the drying.
When adopting sodium hydroxide (highly basic) as reaction raw materials, the chemical equation of this reaction is as follows:
5ZnCl
2+8NaOH+H
2O＝Zn
5(OH)
8Cl
2·H
2O+8NaCl
When adopting ammoniacal liquor (weak base) as reaction raw materials, the chemical equation of this reaction is as follows:
5ZnCl
2+8NH
3·H
2O+H
2O＝Zn
5(OH)
8Cl
2·H
2O+8NH
4Cl
In above-mentioned two kinds of reaction raw materials, more preferably ammoniacal liquor because the relative sodium hydroxide of ammoniacal liquor price is more cheap, has more cost advantage.
In the technique scheme, the mass concentration of said liquor zinci chloridi is preferably 10%～30%.Concentration crosses that low then mother liquor is too many, and energy consumption of reaction increases, and excessive concentration then viscosity is too big, and reaction has some setbacks.
In the technique scheme, the reaction times of said reaction is preferably 0.5h～4h.Through optimal control, can when guaranteeing quality product, improve the efficient of preparation feedback to the reaction times.
In the technique scheme, said rotating speed when centrifugal is preferably 300r/min～1600r/min, and temperature is preferably 80 ℃～120 ℃ when dry,, the water cut that generally is dried to said reaction product is below 10%.
The above-mentioned basic zinc chloride that makes is pulverized, and after packing, can be obtained basic zinc chloride finished product as fodder additives; Zinc content can reach 58%～60% in the finished product, arsenic content≤5ppm, lead content≤5ppm; Cadmium content≤8ppm, the XRD figure spectrum of product is consistent with standard diagram.
Compared with prior art; The invention has the advantages that: under the situation of water that responds, directly react through utilizing zinc chloride and sodium hydroxide or ammoniacal liquor; Need not to add other promotion reagent, reacted product carries out can obtaining basic zinc chloride after spinning, the drying.Preparing method's of the present invention raw material sources are extensive, and by products such as the basic anacidity of product, alkali, the chlorate of generation can further be recycled (for example ammonium chloride evaporation concentration recrystallization capable of using extracts recovery or directly is used for farmland fertilization).Operational path of the present invention is simple, operation easily, and the price of raw materials for production is relatively low, and constant product quality and detrimental impurity content are low, and can satisfy the requirement of environment protection and cleaner production.Than feedstock production basic zinc chlorides such as zinc oxide, useless zinc, zinc subcarbonate, zinc sulfate, the present invention need not to use strong acid such as hydrochloric acid, has reduced the volatilization of severe corrosive gas chlorination hydrogen, helps reducing to corrosion on Equipment; Because the zinc chloride price is more cheap than zinc oxide, zinc carbonate etc., production cost also just more has superiority in addition.
In addition, with the basic zinc chloride feeding animals that the present invention makes, animal not only absorbs soon, and absorption rate is high.
For example: the basic zinc chloride that makes with the present invention feeds pigs as the standard consumption of fodder additives by the zinc source, can promote growth, improves feedstuff-meat ratio, improves yellowish pink, improves its resistance against diseases, and makes the pigskin skin ruddy, the hair color light; Feed piglet and can improve anti-stress ability and the immunizing power of piglet, promote its growth, prevention suckling piglet diarrhea; Feed boar and can prolong the breeding work-ing life of boar;
Basic zinc chloride with the present invention makes is fed poultry as fodder additives by the standard consumption in zinc source, and its speed of growth is improved, and feedstuff-meat ratio descends, and strengthens the feather glossiness, improves its stress ability, reduces mortality ratio;
Basic zinc chloride with the present invention makes is fed aquatic animal as fodder additives by the standard consumption in zinc source, can strengthen its immunizing power, reduces incidence and mortality, promotes to produce, and reduces disease and takes place, and improves efficiency of feed utilization thereby reduce water-soluble loss.
Embodiment
Embodiment 1:
A kind of preparation method of basic zinc chloride of the present invention may further comprise the steps: the first water of interpolation 150ml in the reactor, open whipping appts then; In reactor, drop into the zinc chloride of 20.8g, be warming up to 100 ℃ then, slowly add sodium hydroxide 9.4g again; The pH value is isothermal reaction 2h under 5～9 the condition, and cooling is then stirred cooling with water coolant; Blanking is centrifugal, and centrifugal rotational speed is 1000r/min, go into drying room under 85 ℃, dry to water cut be below 10%; Pulverize 60 mesh sieves, prepared finished product at last.
XRD detection method through routine detects the crystal of finished product to be formed and structure, combines the ultimate principle of chemical reaction simultaneously, can confirm that finished product is a basic zinc chloride.Zinc content is 59.02% in the finished product; Arsenic content is 2.1ppm; Lead content is 3.2ppm; Cadmium content is 2.5ppm, and the XRD figure spectrum of product is consistent with standard diagram, and the assay of zinc content in the finished product and arsenic, lead, cadmium is measured with reference to national standard (GB/T 22546-2008) method of basic zinc chloride.
Embodiment 2:
A kind of preparation method of basic zinc chloride of the present invention may further comprise the steps: the first water of interpolation 300ml in the reactor, open whipping appts then; In reactor, drop into the zinc chloride of 60.0g, be warming up to 65 ℃ then, slowly add the ammoniacal liquor 46g that contains ammonia 26% again; The pH value is isothermal reaction 1h under 5～9 the condition, and cooling is then stirred cooling with water coolant; Blanking is centrifugal, and centrifugal rotational speed is 1100r/min, go into drying room under 95 ℃, dry to water cut below 10%; Pulverize 60 mesh sieves, prepared the basic zinc chloride finished product at last.Zinc content in this finished product is 58.72%, and arsenic content is 1.8ppm, and lead content is 2.2ppm, and cadmium content is 2.9ppm.The detection method of product is identical with embodiment 1.
Embodiment 3:
A kind of preparation method of basic zinc chloride of the present invention may further comprise the steps: the first water of interpolation 1000kg in the reactor, open whipping appts then; In reactor, drop into the zinc chloride of 280kg, be warming up to 80 ℃ then, slowly add the ammoniacal liquor 215kg of ammonia quantity 26% again; The pH value is isothermal reaction 1h under 5～9 the condition, and cooling is then stirred cooling with water coolant; Blanking is centrifugal, and centrifugal rotational speed is 500r/min, go into drying room under 115 ℃, dry to water cut below 10%; Pulverize 60 mesh sieves, prepared the basic zinc chloride finished product at last.Zinc content in this finished product is 58.92%, and arsenic content is 1.5ppm, and lead content is 2.0ppm, and cadmium content is 2.3ppm.The detection method of product is identical with embodiment 1.
Claims (1)
1. preparation method of basic zinc chloride; May further comprise the steps: ammoniacal liquor is added in the liquor zinci chloridi; The mass concentration of said liquor zinci chloridi is 10%～30%; The mol ratio of said ammoniacal liquor and zinc chloride is (7.5～8.5): 5, and be that 60 ℃～105 ℃, pH value are to react 0.5h～4h under 5～9 the condition in temperature, reaction obtains reaction product after accomplishing; With reaction product washing, centrifugal, dry, the rotating speed when centrifugal is 300r/min～1600r/min, and temperature is 70 ℃～120 ℃ when dry, and the water cut that is dried to said reaction product makes basic zinc chloride below 10%.
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|---|---|---|---|
| CN2009103104209A CN101712485B (en) | 2009-11-25 | 2009-11-25 | Preparation method of basic zinc chloride |
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|---|---|---|---|
| CN2009103104209A CN101712485B (en) | 2009-11-25 | 2009-11-25 | Preparation method of basic zinc chloride |
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|---|---|
| CN101712485A CN101712485A (en) | 2010-05-26 |
| CN101712485B true CN101712485B (en) | 2012-06-27 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104108741A (en) * | 2014-07-14 | 2014-10-22 | 上海理工大学 | Preparation method of alkaline zinc chloride particles |
| US9731978B2 (en) | 2014-10-28 | 2017-08-15 | Dongjiang Environmental Co., Ltd. | Method for preparing basic zinc chloride |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102502783B (en) * | 2011-10-14 | 2014-04-02 | 中国科学院上海硅酸盐研究所 | Method for preparing alkali zinc chloride nano-powder in hexagonal flake structures |
| CN102745737B (en) * | 2012-07-27 | 2014-04-09 | 大连交通大学 | Synthesis method of basic zinc chloride monocrystal nanorods |
| CN102976390A (en) * | 2012-12-10 | 2013-03-20 | 常州大学 | Blue-violet fluorescent nano-material and preparation method thereof |
| CN103121706B (en) * | 2013-03-11 | 2014-12-31 | 深圳市危险废物处理站有限公司 | Preparation method of basic zinc chloride |
| CN107324375A (en) * | 2017-06-16 | 2017-11-07 | 河北奥新金属材料科技有限公司 | A kind of preparation method of basic zinc chloride |
| CN110484730A (en) * | 2019-08-14 | 2019-11-22 | 广州科城环保科技有限公司 | A method of recycling feed grade basic zinc chloride from zinc-containing sludge |
| CN110980799B (en) * | 2019-12-26 | 2022-05-31 | 江西省愚人纳米科技有限公司 | Preparation method of basic zinc chloride for feed |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2072191A1 (en) * | 1993-04-05 | 1995-07-01 | Univ Madrid Complutense | Process for obtaining zinc hydroxychloride, Zn5 (OH)8 Cl2.H2O and its use as a zinc corrector |
-
2009
- 2009-11-25 CN CN2009103104209A patent/CN101712485B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2072191A1 (en) * | 1993-04-05 | 1995-07-01 | Univ Madrid Complutense | Process for obtaining zinc hydroxychloride, Zn5 (OH)8 Cl2.H2O and its use as a zinc corrector |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104108741A (en) * | 2014-07-14 | 2014-10-22 | 上海理工大学 | Preparation method of alkaline zinc chloride particles |
| CN104108741B (en) * | 2014-07-14 | 2016-02-03 | 上海理工大学 | A kind of preparation method of basic zinc chloride particle |
| US9731978B2 (en) | 2014-10-28 | 2017-08-15 | Dongjiang Environmental Co., Ltd. | Method for preparing basic zinc chloride |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101712485A (en) | 2010-05-26 |
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Address after: Kang Ning Lu Hunan province 410300 Changsha Changsha Liuyang national biological industry base No. 370 Patentee after: CHANGSHA XINGJIA BIO-ENGINEERING Co.,Ltd. Address before: 1017-1025, room 1, building 410011, Xiang Zhong central 235, Wuyi Road, Hunan, Changsha Patentee before: CHANGSHA XINGJIA BIO-ENGINEERING Co.,Ltd. |