CN110002484A - A kind of preparation method of basicity aluminium polychloride - Google Patents
A kind of preparation method of basicity aluminium polychloride Download PDFInfo
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- CN110002484A CN110002484A CN201910416869.7A CN201910416869A CN110002484A CN 110002484 A CN110002484 A CN 110002484A CN 201910416869 A CN201910416869 A CN 201910416869A CN 110002484 A CN110002484 A CN 110002484A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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Abstract
The invention discloses a kind of preparation methods of basicity aluminium polychloride, more particularly to aluminium polychloride field, the following steps are included: step 1, it will be sequentially added without 60-80 parts and hydrochloric acid 15-20 parts of ammonia distilled water after being heated to 50-60 DEG C into closed reactor, 30-40min is stirred to it in the environment of constant temperature, obtains hydrochloric acid solution;Step 2 is slowly added 20-30 parts of sodium chlorate, after being heated to 40-50 DEG C, magnetic agitation 50-60min into hydrochloric acid solution, after solution is cooled to room temperature, obtains sodium chlorate solution;Sodium chlorate solution is added to closed reactor step 3.The present invention carries out temperature-pressure operation to solution by segmentation, utilize Discrete control temperature, the method for Discrete control strength of fluid, control the concentration of solution in a certain range, effectively control the concentration of concentrate, reduce the possibility of crystallization, crystallization is avoided, the efficiency and yields of production are improved.
Description
Technical field
The present invention relates to aluminium polychloride field, it is more particularly related to a kind of basicity aluminium polychloride
Preparation method.
Background technique
Aluminium polychloride is a kind of emerging water-purifying material, inorganic polymer coagulant, abbreviation poly-aluminium, english abbreviation PAC
(poly aluminum chloride), it be between AlCI3 and Al (OH) 3, between a kind of water-soluble inorganic polyphosphazene polymer
Object is closed, chemical general formula is [Al2 (OH) nCl6-nLm], and wherein m represents extent of polymerization, and n indicates the neutral degree of PAC product.M product
In, n=1-5 is the high charge polymeric rings serobila with structure with Keggin, is had in height electricity to water-borne glue body and particulate matter
With and bridge linking effect, and can strongly remove micro- Toxic and heavy metal ion, character is stablized.
The basis for causing polyaluminium chloride form changeable is OH ion, measures the index of OH ion in polyaluminium chloride salt
Base degree (Basicity is abbreviated as B), is called and does basicity, hydroxide aluminium ratio.Basicity is usually defined as OH in polyaluminium chloride molecule
With the one third of the equivalent percent ((OH)/(Al) × 100 (%)) of Al.It is exactly basicity there are one important indicator,
Influence of the basicity to polyaluminium sulfate be it is direct and objective, it not only influences the fundamental characteristics of polyaluminium sulfate, Er Qie
It must all consider using it as an important indicator in manufacture and use.In the identical raw water of dirty degree, the medicament of investment
It is also in identical situation, the flocculating effect that the different polyaluminium sulfate of basicity generates raw water is different.
Aluminium polychloride in process of production, needs to carry out concentrate drying operation to solution, concentrated using concentration technology
Cheng Zhonghui occurs strength of fluid superelevation and crystallizes, and the steady and continuous for influencing production carries out.
Summary of the invention
In order to overcome the drawbacks described above of the prior art, the embodiment of the present invention provides a kind of system of basicity aluminium polychloride
Preparation Method is carried out temperature-pressure operation to solution by segmentation, is done using Discrete control temperature, Discrete control strength of fluid
Method, the concentration for controlling solution in a certain range, effectively control the concentration of concentrate, reduce the possibility of crystallization, avoid
Crystallization occurs, and improves the efficiency and yields of production.
To achieve the above object, the invention provides the following technical scheme: a kind of preparation method of basicity aluminium polychloride,
The following steps are included:
Step 1 will be sequentially added without 60-80 parts and hydrochloric acid 15-20 parts of ammonia distilled water and will be heated into closed reactor
After 50-60 DEG C, 30-40min is stirred to it in the environment of constant temperature, obtains hydrochloric acid solution;
Step 2 is slowly added 20-30 parts of sodium chlorate, after being heated to 40-50 DEG C into hydrochloric acid solution, magnetic agitation 50-
60min obtains sodium chlorate solution after solution is cooled to room temperature;
Sodium chlorate solution is added to closed reactor step 3, sequentially adds 40-50 parts of aluminium hydroxide, bauxite
After magnetic agitation 20-30min, multiple temperature-pressure operation, stabilization polyaluminium are carried out to it for 10-20 parts and aluminium powder 30-40 part
Aluminium basicity, specific as follows:
First time temperature-pressure:, first slowly will be warm in closed reactor by pressure control in closed reactor in 0.2mpa
Degree is heated up to 70-80 DEG C, then rapid cooling is to keeping the temperature 40-50min after 30-40 DEG C;
Second of temperature-pressure: and then raise pressure in closed reactor to 0.3mpa, first slowly by closed reactor
Interior temperature is heated up to 80-90 DEG C, then rapid cooling is to keeping the temperature 30-40min after 40-50 DEG C;
Third time temperature-pressure: again raising pressure in closed reactor to 0.4mpa, first slowly will be in closed reactor
Temperature is heated up to 90-100 DEG C, then rapid cooling obtains A phase solution to 20-30min is kept the temperature after 50-60 DEG C;
Sodium bicarbonate solution 15-25 parts is added in A phase solution and carries out magnetic agitation 30-40min, then for step 4
In 60 DEG C of at a temperature of polymerization reaction 50-60min, then the solution after reaction is placed in drying box and cures 20-30h, obtains B phase
Solution;
Step 5 filters out the supernatant liquid of B phase solution, obtains aluminium polychloride liquid, the temperature of steam roller is set
It is set to 140-180 DEG C, aluminium polychloride liquid is placed in steam roller and is concentrated and dried, obtains solid powder, then to solid
Body powder is spray-dried, and polyaluminium aluminium powder is obtained;
Polyaluminium aluminium powder is milled by step 6 using flour mill, be made it is evengranular powdered, obtain at
Product.
In a preferred embodiment, in the step 2 and step 3, the revolving speed of magnetic agitation is 80-100
Rev/min, the revolving speed of magnetic agitation is 50-70 revs/min in the step 4.
In a preferred embodiment, in the step 2, when first time temperature-pressure, in closed reactor in
Solution concentration is 16.5%, when second of temperature-pressure, solution concentration 17.5%.
In a preferred embodiment, the temperature setting of drying box is 100-110 DEG C in the step 4.
Technical effect and advantage of the invention:
1, the present invention carries out temperature-pressure operation to solution by segmentation, utilizes Discrete control temperature, Discrete control liquid
The method of concentration, the concentration for controlling solution in a certain range, effectively control the concentration of concentrate, and reduce crystallization can
Can, crystallization is avoided, the efficiency and yields of production are improved.
2, by utilizing controllable temperature heating method, raw material is successively heated, reactive aluminum mistake can be made full use of
The heat released in journey reduces production by the dependence of external heating amount, controls its basicity qualification, stablizes aluminium polychloride alkali
Degree can rationally be produced, effectively be flocculated, during use, the sinking speed of waste is fast, adds according to source water turbidity difference
Amount is lower, can effectively reduce cost.
3, present invention process is simple, and equipment requirement is low, strong operability, has good society generalization application.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1:
A kind of preparation method of basicity aluminium polychloride, comprising the following steps:
Step 1 will be sequentially added without 60 parts and 15 parts of hydrochloric acid of ammonia distilled water after being heated to 50 DEG C into closed reactor,
30min is stirred to it in the environment of constant temperature, obtains hydrochloric acid solution;
Step 2 is slowly added 20 parts of sodium chlorate, after being heated to 40 DEG C into hydrochloric acid solution, 80 revs/min of magnetic agitations
50min obtains sodium chlorate solution after solution is cooled to room temperature;
Sodium chlorate solution is added to closed reactor step 3, sequentially adds 40 parts of aluminium hydroxide, 10 parts of bauxite
With 30 parts of aluminium powder, after 80 revs/min of magnetic agitation 20min, multiple temperature-pressure operation is carried out to it, stablizes polyaluminium aluminium salt
Base degree, specific as follows:
First time temperature-pressure:, first slowly will be warm in closed reactor by pressure control in closed reactor in 0.2mpa
Degree is heated up to 70 DEG C, then rapid cooling is to keeping the temperature 40min after 30 DEG C, in closed reactor in solution concentration control for for
16.5%;
Second of temperature-pressure: and then raise pressure in closed reactor to 0.3mpa, first slowly by closed reactor
Interior temperature is heated up to 80 DEG C, then rapid cooling is to keeping the temperature 30min after 40 DEG C, in closed reactor in solution concentration control be
17.5%;
Third time temperature-pressure: again raising pressure in closed reactor to 0.4mpa, first slowly will be in closed reactor
Temperature is heated up to 90 DEG C, then rapid cooling obtains A phase solution to 20min is kept the temperature after 50 DEG C;
15 parts of sodium bicarbonate solution is added in A phase solution and opens 50 revs/min of magnetic agitation 30min, so for step 4
Afterwards in 60 DEG C of at a temperature of polymerization reaction 50min, then the solution after reaction is placed in the drying box that temperature is 100 DEG C and is cured
20h obtains B phase solution;
Step 5 filters out the supernatant liquid of B phase solution, obtains aluminium polychloride liquid, the temperature of steam roller is set
140 DEG C are set to, aluminium polychloride liquid is placed in steam roller and is concentrated and dried, solid powder is obtained, then to solid powder
End is spray-dried, and polyaluminium aluminium powder is obtained;
Polyaluminium aluminium powder is milled by step 6 using flour mill, be made it is evengranular powdered, obtain at
Product.
Embodiment 2:
A kind of preparation method of basicity aluminium polychloride, comprising the following steps:
Step 1 will be sequentially added without 80 parts and 20 parts of hydrochloric acid of ammonia distilled water after being heated to 60 DEG C into closed reactor,
40min is stirred to it in the environment of constant temperature, obtains hydrochloric acid solution;
Step 2 is slowly added 30 parts of sodium chlorate, after being heated to 50 DEG C into hydrochloric acid solution, 100 revs/min of magnetic agitations
60min obtains sodium chlorate solution after solution is cooled to room temperature;
Sodium chlorate solution is added to closed reactor step 3, sequentially adds 50 parts of aluminium hydroxide, 20 parts of bauxite
With 40 parts of aluminium powder, after 100 revs/min of magnetic agitation 30min, multiple temperature-pressure operation is carried out to it, stablizes aluminium polychloride
Basicity, specific as follows:
First time temperature-pressure:, first slowly will be warm in closed reactor by pressure control in closed reactor in 0.2mpa
Degree is heated up to 80 DEG C, then rapid cooling is to keeping the temperature 50min after 40 DEG C, in closed reactor in solution concentration control for for
16.5%;
Second of temperature-pressure: and then raise pressure in closed reactor to 0.3mpa, first slowly by closed reactor
Interior temperature is heated up to 90 DEG C, then rapid cooling is to keeping the temperature 40min after 50 DEG C, in closed reactor in solution concentration control be
17.5%;
Third time temperature-pressure: again raising pressure in closed reactor to 0.4mpa, first slowly will be in closed reactor
Temperature is heated up to 100 DEG C, then rapid cooling obtains A phase solution to 30min is kept the temperature after 60 DEG C;
25 parts of sodium bicarbonate solution is added in A phase solution and opens 70 revs/min of magnetic agitation 40min, so for step 4
Afterwards in 60 DEG C of at a temperature of polymerization reaction 60min, then the solution after reaction is placed in the drying box that temperature is 110 DEG C and is cured
30h obtains B phase solution;
Step 5 filters out the supernatant liquid of B phase solution, obtains aluminium polychloride liquid, the temperature of steam roller is set
180 DEG C are set to, aluminium polychloride liquid is placed in steam roller and is concentrated and dried, solid powder is obtained, then to solid powder
End is spray-dried, and polyaluminium aluminium powder is obtained;
Polyaluminium aluminium powder is milled by step 6 using flour mill, be made it is evengranular powdered, obtain at
Product.
Embodiment 3:
A kind of preparation method of basicity aluminium polychloride, comprising the following steps:
Step 1 will be sequentially added without 70 parts and 17 parts of hydrochloric acid of ammonia distilled water after being heated to 55 DEG C into closed reactor,
35min is stirred to it in the environment of constant temperature, obtains hydrochloric acid solution;
Step 2 is slowly added 25 parts of sodium chlorate, after being heated to 45 DEG C into hydrochloric acid solution, 90 revs/min of magnetic agitations
55min obtains sodium chlorate solution after solution is cooled to room temperature;
Sodium chlorate solution is added to closed reactor step 3, sequentially adds 45 parts of aluminium hydroxide, 15 parts of bauxite
With 35 parts of aluminium powder, after 90 revs/min of magnetic agitation 25min, multiple temperature-pressure operation is carried out to it, stablizes polyaluminium aluminium salt
Base degree, specific as follows:
First time temperature-pressure:, first slowly will be warm in closed reactor by pressure control in closed reactor in 0.2mpa
Degree is heated up to 75 DEG C, then rapid cooling is to keeping the temperature 45min after 35 DEG C, in closed reactor in solution concentration control for for
16.5%;
Second of temperature-pressure: and then raise pressure in closed reactor to 0.3mpa, first slowly by closed reactor
Interior temperature is heated up to 85 DEG C, then rapid cooling is to keeping the temperature 35min after 45 DEG C, in closed reactor in solution concentration control be
17.5%;
Third time temperature-pressure: again raising pressure in closed reactor to 0.4mpa, first slowly will be in closed reactor
Temperature is heated up to 95 DEG C, then rapid cooling obtains A phase solution to 25min is kept the temperature after 55 DEG C;
20 parts of sodium bicarbonate solution is added in A phase solution and opens 60 revs/min of magnetic agitation 35min, so for step 4
Afterwards in 60 DEG C of at a temperature of polymerization reaction 55min, then the solution after reaction is placed in the drying box that temperature is 115 DEG C and is cured
25h obtains B phase solution;
Step 5 filters out the supernatant liquid of B phase solution, obtains aluminium polychloride liquid, the temperature of steam roller is set
160 DEG C are set to, aluminium polychloride liquid is placed in steam roller and is concentrated and dried, solid powder is obtained, then to solid powder
End is spray-dried, and polyaluminium aluminium powder is obtained;
Polyaluminium aluminium powder is milled by step 6 using flour mill, be made it is evengranular powdered, obtain at
Product.
Embodiment 4:
A kind of preparation method of basicity aluminium polychloride, comprising the following steps:
Step 1 will be sequentially added without 80 parts and 20 parts of hydrochloric acid of ammonia distilled water after being heated to 60 DEG C into closed reactor,
40min is stirred to it in the environment of constant temperature, obtains hydrochloric acid solution;
Step 2 is slowly added 20 parts of sodium chlorate, after being heated to 40 DEG C into hydrochloric acid solution, 80 revs/min of magnetic agitations
50min obtains sodium chlorate solution after solution is cooled to room temperature;
Sodium chlorate solution is added to closed reactor step 3, sequentially adds 50 parts of aluminium hydroxide, 20 parts of bauxite
With 40 parts of aluminium powder, after 80 revs/min of magnetic agitation 20min, multiple temperature-pressure operation is carried out to it, stablizes polyaluminium aluminium salt
Base degree, specific as follows:
First time temperature-pressure:, first slowly will be warm in closed reactor by pressure control in closed reactor in 0.2mpa
Degree is heated up to 75 DEG C, then rapid cooling is to keeping the temperature 45min after 35 DEG C, in closed reactor in solution concentration control for for
16.5%;
Second of temperature-pressure: and then raise pressure in closed reactor to 0.3mpa, first slowly by closed reactor
Interior temperature is heated up to 85 DEG C, then rapid cooling is to keeping the temperature 35min after 45 DEG C, in closed reactor in solution concentration control be
17.5%;
Third time temperature-pressure: again raising pressure in closed reactor to 0.4mpa, first slowly will be in closed reactor
Temperature is heated up to 95 DEG C, then rapid cooling obtains A phase solution to 25min is kept the temperature after 55 DEG C;
15 parts of sodium bicarbonate solution is added in A phase solution and opens 60 revs/min of magnetic agitation 35min, so for step 4
Afterwards in 60 DEG C of at a temperature of polymerization reaction 55min, then the solution after reaction is placed in the drying box that temperature is 115 DEG C and is cured
25h obtains B phase solution;
Step 5 filters out the supernatant liquid of B phase solution, obtains aluminium polychloride liquid, the temperature of steam roller is set
160 DEG C are set to, aluminium polychloride liquid is placed in steam roller and is concentrated and dried, solid powder is obtained, then to solid powder
End is spray-dried, and polyaluminium aluminium powder is obtained;
Polyaluminium aluminium powder is milled by step 6 using flour mill, be made it is evengranular powdered, obtain at
Product.
By the available four kinds of basicity aluminium polychlorides of above four groups of embodiments, these four aluminium polychlorides are distinguished
It is tested for the property, then is tested for the property with the aluminium polychloride Jing Guo common process, as a result obtained in four groups of embodiments
The performance of aluminium polychloride has different promotions, and wherein the performance of aluminium polychloride is best in embodiment 3, is worth highest, leads to
It crosses segmentation and temperature-pressure operation is carried out to solution, using Discrete control temperature, the method for Discrete control strength of fluid, control solution
Concentration in a certain range, effectively control the concentration of concentrate, reduce the possibility of crystallization, avoid crystallization, mention
The high efficiency and yields of production successively heats raw material using controllable temperature heating method, can be abundant
It using the heat released during reactive aluminum, reduces production by the dependence of external heating amount, controls its basicity qualification, stablize poly-
Aluminium chloride basicity is closed, can rationally produce, effectively flocculate according to source water turbidity difference, during use, the sedimentation of waste
Speed is fast, and dosage is lower, can effectively reduce cost.
Table 1 is each component ingredient accounting table of comparisons in embodiment 1-5.
Table 2 is the finished product items underlying parameter table of comparisons in embodiment 1-5.
Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
Basicity B (%) | 83.45 | 85.85 | 87.35 | 86.55 |
PH value | 3.5-4.0 | 3.5-4.0 | 3.5-5.0 | 3.5-5.0 |
Water insoluble substance (%) | 0.65 | 0.85 | 0.50 | 0.60 |
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features,
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (4)
1. a kind of preparation method of basicity aluminium polychloride, which comprises the following steps:
Step 1 will sequentially add without 60-80 parts and hydrochloric acid 15-20 parts of ammonia distilled water and be heated to 50-60 into closed reactor
After DEG C, 30-40min is stirred to it in the environment of constant temperature, obtains hydrochloric acid solution;
Step 2 is slowly added 20-30 parts of sodium chlorate, after being heated to 40-50 DEG C into hydrochloric acid solution, magnetic agitation 50-
60min obtains sodium chlorate solution after solution is cooled to room temperature;
Sodium chlorate solution is added to closed reactor step 3, sequentially adds 40-50 parts of aluminium hydroxide, bauxite 10-20
Part and aluminium powder 30-40 part, after magnetic agitation 20-30min, multiple temperature-pressure operation, stabilization polyaluminium aluminium salt are carried out to it
Base degree, specific as follows:
First time temperature-pressure: pressure control in closed reactor is first slowly added confined reaction temperature in the kettle in 0.2mpa
Temperature is to 70-80 DEG C, then rapid cooling is to keeping the temperature 40-50min after 30-40 DEG C;
Second of temperature-pressure: and then raise pressure in closed reactor to 0.3mpa, it first slowly will be warm in closed reactor
Degree is heated up to 80-90 DEG C, then rapid cooling is to keeping the temperature 30-40min after 40-50 DEG C;
Third time temperature-pressure: pressure in closed reactor is raised to 0.4mpa, first slowly by confined reaction temperature in the kettle again
It is heated up to 90-100 DEG C, then rapid cooling obtains A phase solution to 20-30min is kept the temperature after 50-60 DEG C;
Sodium bicarbonate solution 15-25 parts is added in A phase solution and carries out magnetic agitation 30-40min, then 60 for step 4
Polymerization reaction 50-60min at a temperature of DEG C, then the solution after reaction is placed in drying box and cures 20-30h, it obtains B and mixes
Liquid;
Step 5 filters out the supernatant liquid of B phase solution, obtains aluminium polychloride liquid, is by the temperature setting of steam roller
140-180 DEG C, aluminium polychloride liquid is placed in steam roller and is concentrated and dried, solid powder is obtained, then to solid powder
End is spray-dried, and polyaluminium aluminium powder is obtained;
Polyaluminium aluminium powder is milled by step 6 using flour mill, and evengranular powdered, acquisition finished product is made.
2. a kind of preparation method of basicity aluminium polychloride according to claim 1, it is characterised in that: the step 2
In step 3, the revolving speed of magnetic agitation is 80-100 revs/min, and the revolving speed of magnetic agitation is 50-70 in the step 4
Rev/min.
3. a kind of preparation method of basicity aluminium polychloride according to claim 1, it is characterised in that: the step 2
In, when first time temperature-pressure, in closed reactor in solution concentration control be 16.5%, it is molten when second of temperature-pressure
The control of liquid concentration is 17.5%.
4. a kind of preparation method of basicity aluminium polychloride according to claim 1, it is characterised in that: the step 4
The temperature setting of middle drying box is 100-110 DEG C.
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CN101549879A (en) * | 2009-05-12 | 2009-10-07 | 苏州市亨文环保水业有限公司 | Production method of polyaluminium chloride |
CN101591032A (en) * | 2009-06-29 | 2009-12-02 | 同济大学 | The method for preparing modified polyaluminium chloride flocculating agent with the depleted molecular sieve |
CN106186020A (en) * | 2016-07-07 | 2016-12-07 | 杭州萧山三江净水剂有限公司 | A kind of preparation method of the aluminium polychlorid of high basicity high concentration |
CN106186019A (en) * | 2016-07-07 | 2016-12-07 | 杭州萧山三江净水剂有限公司 | A kind of preparation method of the aluminium polychlorid of low-residue aluminum |
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- 2019-05-20 CN CN201910416869.7A patent/CN110002484B/en active Active
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EP1151965A2 (en) * | 2000-05-02 | 2001-11-07 | Sachtleben Chemie GmbH | Process for the preparation of polyaluminium nitrates and their use in water purification |
CN101549879A (en) * | 2009-05-12 | 2009-10-07 | 苏州市亨文环保水业有限公司 | Production method of polyaluminium chloride |
CN101591032A (en) * | 2009-06-29 | 2009-12-02 | 同济大学 | The method for preparing modified polyaluminium chloride flocculating agent with the depleted molecular sieve |
CN106186020A (en) * | 2016-07-07 | 2016-12-07 | 杭州萧山三江净水剂有限公司 | A kind of preparation method of the aluminium polychlorid of high basicity high concentration |
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