CN116282109A - Preparation method of polyaluminum chloride for papermaking sizing agent - Google Patents

Preparation method of polyaluminum chloride for papermaking sizing agent Download PDF

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Publication number
CN116282109A
CN116282109A CN202310243738.XA CN202310243738A CN116282109A CN 116282109 A CN116282109 A CN 116282109A CN 202310243738 A CN202310243738 A CN 202310243738A CN 116282109 A CN116282109 A CN 116282109A
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Prior art keywords
sodium carbonate
polyaluminum chloride
product
chloride product
crude
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CN202310243738.XA
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Chinese (zh)
Inventor
史立达
王磊
李浩列
王昌义
王婷
赵艳爽
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Chalco Shandong Co ltd
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Chalco Shandong Co ltd
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Priority to CN202310243738.XA priority Critical patent/CN116282109A/en
Publication of CN116282109A publication Critical patent/CN116282109A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/48Halides, with or without other cations besides aluminium
    • C01F7/56Chlorides
    • C01F7/57Basic aluminium chlorides, e.g. polyaluminium chlorides
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/16Sizing or water-repelling agents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/64Paper recycling

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The application relates to the technical field of chemical synthesis, in particular to a preparation method of polyaluminium chloride for a papermaking sizing agent; the preparation method comprises the following steps: under the normal pressure condition, reacting aluminum hydroxide with byproduct hydrochloric acid to a preset temperature, and then performing first heat preservation to obtain a crude polyaluminium chloride product; adding sodium carbonate into the polyaluminum chloride crude product for adjustment, then carrying out second heat preservation, and then filtering to obtain a polyaluminum chloride product; wherein the added amount of the sodium carbonate is in direct proportion to the target basicity of the polyaluminum chloride product; firstly, aluminum hydroxide and byproduct hydrochloric acid are utilized to react under normal pressure to generate a crude polyaluminium chloride product, then sodium carbonate is added to adjust and remove impurities in the crude polyaluminium chloride product, sodium and carbonate impurities introduced by adding sodium carbonate can be removed in a way of precipitation crystallization, a polyaluminium chloride product with high basicity can be obtained, and then the polyaluminium chloride product with high purity and high basicity can be obtained through filtration.

Description

Preparation method of polyaluminum chloride for papermaking sizing agent
Technical Field
The application relates to the technical field of chemical synthesis, in particular to a preparation method of polyaluminium chloride for a papermaking sizing agent.
Background
Neutral sizing agents are currently popular processes in the paper industry for a number of advantages, in that polyaluminum chloride is often used as a precipitant in neutral sizing agents because it can both adjust the pH to neutral and is an effective source of aluminum that has a positive charge under neutral conditions. However, because the conventional polyaluminium chloride product has more impurities, the conventional polyaluminium chloride product can be directly used in the papermaking sizing process to have adverse effect on the papermaking quality, so that the high-purity polyaluminium chloride product is usually synthesized by adopting aluminum hydroxide and high-purity hydrochloric acid through a pressurized acid dissolution one-step method at present, and the synthesized polyaluminium chloride product is used as a papermaking sizing agent.
But is limited by the one-step process limitations of pressurized acid dissolution, the basicity of polyaluminum chloride products used in the commercial production for sizing paper is not higher than 60%, whereas the color and luster of pure liquid polyaluminum chloride varies with the basicity size: when the basicity is 40% -60%, the liquid is light yellow transparent liquid; when the basicity is above 60%, the liquid is colorless transparent liquid; and the raw materials contain a certain amount of impurities, and the impurities enter the solution in the process of dissolving out the raw materials, so that the papermaking quality is affected. Therefore, the polyaluminium chloride product produced by the pressurized acid-soluble one-step process cannot be directly applied to the papermaking sizing agent, so that the polyaluminium chloride product produced by the process is generally pretreated by activated carbon, impurities in the polyaluminium chloride product are removed by adsorption, otherwise, the papermaking quality is affected, but the used activated carbon belongs to dangerous waste, environmental pollution is easy to cause, and the running cost is increased by subsequent treatment; therefore, how to provide a preparation method of polyaluminum chloride without activated carbon adsorption is a technical problem which needs to be solved at present.
Disclosure of Invention
The application provides a preparation method of polyaluminium chloride for a papermaking sizing agent, which aims to solve the technical problem that the polyaluminium chloride produced by adopting a pressurized acid dissolution one-step process in the prior art can be used for the papermaking sizing agent only by adopting activated carbon adsorption.
In a first aspect, the present application provides a method for preparing polyaluminium chloride for a papermaking sizing agent, the method comprising:
under the normal pressure condition, reacting aluminum hydroxide with byproduct hydrochloric acid to a preset temperature, and then performing first heat preservation to obtain a crude polyaluminium chloride product;
adding sodium carbonate into the polyaluminum chloride crude product for adjustment, then carrying out second heat preservation, and then filtering to obtain a polyaluminum chloride product;
wherein the added amount of sodium carbonate is in direct proportion to the target basicity of the polyaluminum chloride product.
Optionally, the addition amount m of the sodium carbonate and the target basicity n of the polyaluminum chloride product satisfy:
m=2.26n+2.69。
optionally, the target basicity is more than or equal to 60%.
Optionally, the preset temperature is 100 ℃ ± 5 ℃.
Optionally, the first heat preservation time is more than or equal to 1h.
Optionally, the second heat preservation time is 0.5 h-1 h.
Optionally, the sodium carbonate is added in a manner of rapidly stirring the crude polyaluminum chloride product, and the rapid stirring speed is 200 r/min-500 r/min.
Optionally, the rapid stirring time is 0.5-5 h.
Optionally, the purity of the byproduct hydrochloric acid is 27% -34%.
In a second aspect, the present application provides a papermaking sizing agent comprising polyaluminum chloride obtained by the method of preparation of the first aspect.
Compared with the prior art, the technical scheme provided by the embodiment of the application has the following advantages:
according to the preparation method of the polyaluminium chloride for the papermaking sizing agent, which is provided by the embodiment of the application, aluminum hydroxide and byproduct hydrochloric acid are utilized to react under normal pressure, first heat preservation is carried out, so that aluminum hydroxide and byproduct hydrochloric acid can be guaranteed to generate a polyaluminium chloride crude product, sodium carbonate is added to adjust, the characteristic that an aqueous solution of sodium carbonate is alkaline is utilized, impurities in the polyaluminium chloride crude product can be precipitated, the impurities in the polyaluminium chloride crude product can be further removed through the characteristic of sodium salt, sodium and carbonate impurities introduced by adding sodium carbonate can be removed through a crystallization separation mode, a polyaluminium chloride product with high basicity can be obtained, and then filtration is carried out, so that the polyaluminium chloride product with high purity and high basicity can be obtained.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the application and together with the description, serve to explain the principles of the application.
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required to be used in the description of the embodiments or the prior art will be briefly described below, and it will be obvious to those skilled in the art that other drawings can be obtained from these drawings without inventive effort.
Fig. 1 is a schematic flow chart of a preparation method provided in an embodiment of the present application.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
Unless specifically indicated otherwise, the various raw materials, reagents, instruments, equipment, and the like used in this application are commercially available or may be prepared by existing methods.
The inventive thinking of this application is:
the high-purity polyaluminium chloride used for the sizing agent for papermaking is synthesized by taking aluminum hydroxide and high-purity hydrochloric acid as raw materials under a one-step process of pressurized acid dissolution. Meanwhile, the reaction conditions are that the high temperature and the high pressure are severe, a special F-shaped enamel reaction kettle is needed, the equipment has high cost and short service life, and the service life is generally about three years; in addition, the maintenance cost of the F-shaped enamel reaction kettle is high, so that the production cost is increased.
In addition, the polyaluminum chloride produced by adopting aluminum hydroxide and high-purity hydrochloric acid through a pressurized acid dissolution one-step method contains certain impurities, the impurities are required to be removed by adopting activated carbon adsorption, the activated carbon becomes solid waste after being used, environmental pollution is easy to cause in the stacking, storage and transportation processes, and the post-treatment increases the production cost.
Therefore, how to provide a preparation method of polyaluminum chloride without activated carbon adsorption is a technical problem which needs to be solved at present.
As shown in fig. 1, an embodiment of the present application provides a method for preparing polyaluminum chloride for a papermaking sizing agent, the method comprising:
s1, under the normal pressure condition, reacting aluminum hydroxide with byproduct hydrochloric acid to a preset temperature, and then carrying out first heat preservation to obtain a crude polyaluminium chloride product;
s2, adding sodium carbonate into the polyaluminum chloride crude product for adjustment, then carrying out second heat preservation, and then filtering to obtain a polyaluminum chloride product;
wherein the added amount of sodium carbonate is in direct proportion to the target basicity of the polyaluminum chloride product.
In some alternative embodiments, the addition m of sodium carbonate and the target basicity n of the polyaluminum chloride product satisfy between:
m=2.26n+2.69。
in the embodiment of the application, the relation between the adding amount of sodium carbonate and the target basicity of the polyaluminum chloride product is limited, so that the sodium carbonate can act as the adjusting effect of the regulator, impurities in the polyaluminum chloride crude product can be precipitated by the sodium carbonate, and the pure polyaluminum chloride product is obtained.
In some alternative embodiments, the target basicity is ≡60%.
In the embodiment of the application, the positive effect of limiting the target basicity to be more than or equal to 60 percent is that the purity in the final polyaluminum chloride product can be ensured to meet the expectations within the scope of the basicity, and meanwhile, the adding amount of sodium carbonate is ensured to be enough, so that the pure polyaluminum chloride product is obtained.
In some alternative embodiments, the preset temperature is 100 ℃ ± 5 ℃.
In the embodiment of the application, the positive effect of limiting the preset temperature to be 100+/-5 ℃ is that in the temperature range, as the reaction of the aluminum hydroxide and the byproduct hydrochloric acid is a heating reaction, the reaction between the aluminum hydroxide and the byproduct hydrochloric acid can be completely demonstrated in the preset temperature range, so that enough polyaluminium chloride crude products can be obtained.
In some alternative embodiments, the first incubation time is greater than or equal to 1 hour.
In the embodiment of the application, the positive effect of limiting the first heat preservation time to be more than or equal to 1h is that the reaction between the aluminum hydroxide and the byproduct hydrochloric acid can be ensured to be sufficient in the time range, so that enough crude polyaluminium chloride products are obtained.
In some alternative embodiments, the second incubation time is from 0.5h to 1h.
In the embodiment of the application, the positive effect of limiting the second heat preservation time to be 0.5-1 h is that in the time range, the characteristic that the sodium carbonate aqueous solution is alkaline is utilized, so that impurities in the crude product of polyaluminum chloride can be precipitated, the impurities in the crude product of polyaluminum chloride can be further removed through the characteristic of sodium salt, sodium and carbonate impurities introduced by adding sodium carbonate can be removed through a crystallization separation mode, and the regulation effect of sodium carbonate serving as a regulator is ensured.
In some alternative embodiments, the sodium carbonate is added by rapid stirring of the crude polyaluminum chloride product at a speed of 200r/min to 500r/min.
In this application embodiment, inject the rotational speed of mode and the rapid mixing of sodium carbonate, through the mode of rapid mixing, can guarantee to mix fully between polyaluminum chloride crude product and the sodium carbonate to guarantee the regulation effect of sodium carbonate.
In some alternative embodiments, the rapid agitation is for a period of time ranging from 0.5h to 5h.
In this application embodiment, inject the concrete time of rapid mixing, can guarantee the stirring effect of rapid mixing for mix fully between polyaluminum chloride crude product and the sodium carbonate, thereby guarantee the regulation effect of sodium carbonate.
In some alternative embodiments, the byproduct hydrochloric acid has a purity of 27% to 34%.
In the embodiment of the application, the purity of the byproduct hydrochloric acid is limited to be 27% -34%, and the positive effect is that in the purity range, enough HCl in the byproduct hydrochloric acid can be ensured, so that the reaction of aluminum hydroxide and the byproduct hydrochloric acid is ensured to be sufficient, and enough polyaluminium chloride crude products are obtained.
Based on one general inventive concept, embodiments of the present application provide a paper sizing agent including polyaluminum chloride obtained by the preparation method.
The papermaking sizing agent is realized based on the preparation method, the specific steps of the preparation method can refer to the embodiment, and as the papermaking sizing agent adopts part or all of the technical schemes of the embodiment, the papermaking sizing agent has at least all the beneficial effects brought by the technical schemes of the embodiment, and the detailed description is omitted.
The present application is further illustrated below in conjunction with specific examples. It should be understood that these examples are illustrative only of the present application and are not intended to limit the scope of the present application. The experimental procedures, which are not specified in the following examples, are generally determined according to national standards. If the corresponding national standard does not exist, the method is carried out according to the general international standard, the conventional condition or the condition recommended by the manufacturer.
Example 1
The preparation method specifically comprises the following steps:
adding aluminum hydroxide and byproduct hydrochloric acid into a beaker, starting stirring and heating to 100 ℃, and then preserving heat for 1h; according to the target basicity, adding a certain amount of sodium carbonate regulator in a rapid stirring state, and preserving heat for 0.5-1 h after the addition of the sodium carbonate regulator is finished. And then filtering to obtain the high-basicity high-purity polyaluminum chloride.
Example 2
Example 2 and example 1 were compared, and the difference between example 2 and example 1 is that:
examples of single experiments with treatment: according to the method, aluminum hydroxide and byproduct hydrochloric acid are reacted to obtain crude aluminum chloride product solution. After each experiment, 300g of aluminum chloride solution was weighed, and sodium carbonate modifier was added according to the target basicity as shown in table 1, respectively, followed by suction filtration to obtain polyaluminum chloride product.
Table 1 table of the charging conditions
Sequence number Aluminum chloride mass (g) Sodium carbonate mass (g) Target basicity (%)
1 300 25.38 60
2 300 27.6 65
3 300 29.81 70
4 300 34.24 80
The basicity of the resulting polyaluminum chloride product in each experiment was separately measured and the results are shown in table 2.
TABLE 2 basicity of polyaluminum chloride products
Sequence number Detection of basicity (%)
1 60.53
2 66.02
3 69.89
4 80.43
Specific analysis of table 2:
as can be seen from the data in table 2, the sodium carbonate modifier is generally added to the product of the reaction between aluminum hydroxide and byproduct hydrochloric acid under normal pressure, so as to directly obtain high-purity polyaluminum chloride suitable for the papermaking sizing agent, thereby not only reducing the use of activated carbon, but also obtaining a polyaluminum chloride product with high basicity and high purity.
One or more technical solutions in the embodiments of the present application at least further have the following technical effects or advantages:
(1) According to the preparation method of the polyaluminum chloride for the papermaking sizing agent, sodium carbonate is used as a regulator, added into an aluminum trichloride solution generated by the reaction of byproduct hydrochloric acid and aluminum hydroxide under normal pressure, and reacted under normal temperature stirring, impurities are removed in the process of crystallization and precipitation of generated sodium salt, so that the polyaluminum chloride with high basicity is obtained, and therefore, for the papermaking industry, the production link of activated carbon adsorption is not needed, and the production of hazardous waste in the traditional papermaking industry and the adverse effect on the environment are reduced.
(2) According to the preparation method of the polyaluminium chloride for the papermaking sizing agent, provided by the embodiment of the application, the polyaluminium chloride applicable to the papermaking sizing agent can be directly obtained under normal pressure by using the aluminum hydroxide and the byproduct hydrochloric acid, so that innovation of a high-purity low-iron polyaluminium chloride production process is realized, and meanwhile, investment of equipment cost is reduced.
(3) The preparation method of the polyaluminium chloride for the papermaking sizing agent can realize production process transformation in the polyaluminium chloride industry, has great promotion significance for clean production in the papermaking industry, and improves the production technical level of the industry.
Various embodiments of the present application may exist in a range format; it should be understood that the description in a range format is merely for convenience and brevity and should not be interpreted as a rigid limitation on the scope of the application. It is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
In this application, unless otherwise indicated, terms of orientation such as "upper" and "lower" are used specifically to refer to the orientation of the drawing in the figures. In addition, in the description of the present application, the terms "include", "comprise", "comprising" and the like mean "including but not limited to".
Relational terms such as "first" and "second", and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Herein, "and/or" describing an association relationship of an association object means that there may be three relationships, for example, a and/or B, may mean: a alone, a and B together, and B alone. Wherein A, B may be singular or plural. Herein, "at least one" means one or more, and "a plurality" means two or more. "at least one", "at least one" or the like refer to any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
The foregoing is merely a specific embodiment of the application to enable one skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. A method for preparing polyaluminium chloride for a papermaking sizing agent, which is characterized by comprising the following steps:
under the normal pressure condition, reacting aluminum hydroxide with byproduct hydrochloric acid to a preset temperature, and then performing first heat preservation to obtain a crude polyaluminium chloride product;
adding sodium carbonate into the polyaluminum chloride crude product for adjustment, then carrying out second heat preservation, and then filtering to obtain a polyaluminum chloride product;
wherein the added amount of sodium carbonate is in direct proportion to the target basicity of the polyaluminum chloride product.
2. The preparation method according to claim 1, wherein the addition amount m of sodium carbonate and the target basicity n of the polyaluminum chloride product satisfy:
m=2.26n+2.69。
3. the method of claim 1 or 2, wherein the target basicity is not less than 60%.
4. The method of claim 1, wherein the predetermined temperature is 100 ℃ ± 5 ℃.
5. The method according to claim 1, wherein the first incubation time is not less than 1 hour.
6. The method according to claim 1, wherein the second incubation time is 0.5h to 1h.
7. The method according to claim 1, wherein the sodium carbonate is added by rapid stirring of the crude polyaluminum chloride product at a rotational speed of 200r/min to 500r/min.
8. The method of claim 7, wherein the rapid stirring time is 0.5 to 5 hours.
9. The method according to claim 1, wherein the purity of the by-product hydrochloric acid is 27% -34%.
10. A paper sizing agent comprising polyaluminum chloride obtained by the process according to any one of claims 1 to 9.
CN202310243738.XA 2023-03-10 2023-03-10 Preparation method of polyaluminum chloride for papermaking sizing agent Pending CN116282109A (en)

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CN202310243738.XA CN116282109A (en) 2023-03-10 2023-03-10 Preparation method of polyaluminum chloride for papermaking sizing agent

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Application Number Priority Date Filing Date Title
CN202310243738.XA CN116282109A (en) 2023-03-10 2023-03-10 Preparation method of polyaluminum chloride for papermaking sizing agent

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