CN105948069A - Preparation method of activated clay loaded sodium hydroxide - Google Patents

Preparation method of activated clay loaded sodium hydroxide Download PDF

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Publication number
CN105948069A
CN105948069A CN201610260163.2A CN201610260163A CN105948069A CN 105948069 A CN105948069 A CN 105948069A CN 201610260163 A CN201610260163 A CN 201610260163A CN 105948069 A CN105948069 A CN 105948069A
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filter cake
prepares
preparation
active hargil
stirring
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Inventor
梁福珏
梁福瑜
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Longan Guangxi Rui Feng Trade Co Ltd
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Longan Guangxi Rui Feng Trade Co Ltd
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Priority to CN201610260163.2A priority Critical patent/CN105948069A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/36Silicates having base-exchange properties but not having molecular sieve properties
    • C01B33/38Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
    • C01B33/40Clays

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
  • Treatment Of Sludge (AREA)

Abstract

The invention discloses a preparation method of an activated clay loaded sodium hydroxide, and belongs to the technical field of bentonite deep processing. The activated clay loaded sodium hydroxide is prepared by the steps such as preparation of material, slurrying, acid activation reaction, filter pressing, alkalization, drying, and crushing. The alkali capacity of the activated clay loaded sodium hydroxide prepared by the invention is 19-19.4mmol/g, and the quality is stable. The added reducing agent in the invention can reduce the Fe<3+> generated by an acid corrosion device to the Fe<2+> having light color, and the influence on the whiteness of the activated clay caused by the color of Fe<3+> is avoided.

Description

A kind of preparation method of load hydrogen sodium oxide active hargil
[technical field]
The invention belongs to bentonite deep process technology field, be specifically related to a kind of load hydrogen sodium oxide active hargil Preparation method.
[background technology]
Bentonite is referred to as natural nano-material, general-purpose clay.China's bentonite is best in quality, and ore reserves occupies the world Second, in addition to exporting as bentonite raw material on a small quantity, remaining is all with bentonite in powder and active hargil shape Formula marketing is domestic, and these products belong to primary product, and economic benefit is the highest, and level of resource utilization is low.In order to obtain Bigger economic benefit, needs to develop the seriation new product of high-tech content, expansive approach frontier.
Load hydrogen sodium oxide active hargil is with bentonite as raw material, acidified after form active hargil, at this base Re-boostering test on plinth and obtain, it is a kind of lamellar mineral materials, has special anion-exchange capacity.It is permissible It is directly used in the purification of the deacidification of the food liquid such as fruit juice, vegetable oil, decolouring and drainage, air and water quality, urges The preparation etc. of agent, it is also possible to the nano material that organic acid reaction prepares NEW TYPE OF COMPOSITE stratiform, for coating, The field such as plastics and novel absorption material.But the prior art of industrialized production load hydrogen sodium oxide active hargil In to there is the quality of production, efficiency low and unstable, the cycle is long, high in cost of production problem, therefore, how to improve Load hydrogen sodium oxide activated clay production quality, stability, efficiency, reduce cost, become bentonite and deeply add One important directions of work research.
Patent Application Publication " preparation method of a kind of loaded calcium hydroxide activity carclazyte (application number: 201510081886.1) preparation method of a kind of loaded calcium hydroxide activity carclazyte, described load " are disclosed Calcium hydroxide activity carclazyte is through dispensing slurrying, acid activation reaction, filter pressing for the first time, washing and second time pressure Prepared by the steps such as filter, alkalization, filter pressing for the third time, dry, pulverizing, the load hydrogen-oxygen that the method is produced Change calcium active hargil and there is the shortcomings such as whiteness is the highest, alkali capacity is low, quality is unstable.
[summary of the invention]
The technical problem to be solved in the present invention is to provide the preparation method of a kind of load hydrogen sodium oxide active hargil, with Solve load hydrogen sodium oxide active hargil in prior art and have that whiteness is the highest, alkali capacity is low, quality is unstable Problem.Load hydrogen sodium oxide active hargil steady quality, alkali capacity prepared by the present invention are high.
For solve above technical problem, the present invention by the following technical solutions:
The preparation method of a kind of load hydrogen sodium oxide active hargil, comprises the following steps:
S1: by bentonite and active hargil waste water that concentration is 13%-16% by weight for 1.6-2.2:10-14 Mixing, stirs under the conditions of rotating speed is 200-500r/min, prepares pasty material A;
S2: the pasty material A that step S1 prepares is joined in the inorganic mixed acid that concentration is 11%-20%, Described inorganic mixed acid is the sulphuric acid of concentration 16-18wt%, the carbonic acid of concentration 32-36wt%, concentration 18-20wt% The mixed acid of oxalic acid 2-6:3-5:2-3 by volume composition, the weight ratio of pasty material A and inorganic mixed acid For 1-3.2:4-16, under the conditions of rotating speed is 200-550r/min, add ammonium sulfide stirring, ammonium sulfide and slurry The weight ratio of material A is 1-2:50-150, is heated to 82-93 DEG C, reacts 1.2-3.2h under the conditions of being maintained at 82-93 DEG C, Prepare pasty material B;
S3: the pasty material B that step S2 prepares is carried out filter pressing under the conditions of pressure is 0.9-0.95MPa, Prepared moisture content is the filter cake A of 32%-45%;
S4: the filter cake A prepared to step S3 adds water stirring and dissolving, and amount of water is the 6-7.5 of filter cake A weight Times, stirring and dissolving filter cake A adds flocculant stirring 0.4-1.2h after completing makes solution precipitate, by precipitate in pressure Power is to carry out filter pressing under the conditions of 0.9-0.95MPa, and prepared moisture content is the filter cake B of 32%-45%;
S5: add water stirring and dissolving by the filter cake B that step S4 prepares, and amount of water is the 5-6.5 of filter cake B weight Times, after stirring and dissolving filter cake B completes, add sodium hydroxide solution, prepare slurry material C;
S6: the slurry material C that step S5 prepares is carried out filter pressing under the conditions of pressure is 0.9-0.95MPa, system Obtain the filter cake C that moisture content is 32%-45%;
S7: the filter cake C that step S6 prepares is placed in centrifuge and removes water to powder after filter cake C moisture content≤5% Broken, gained ground product sieves, and prepares load hydrogen sodium oxide active hargil.
Further, the one during flocculant described in step S4 includes organic flocculant and inorganic flocculating agent.
Further, during described organic flocculant includes sodium polyacrylate, calcium polyacrylate (CPA), acrylamide Kind.
Further, one or more during described inorganic flocculating agent includes bodied ferric sulfate, polyaluminium sulfate.
Further, concentration of sodium hydroxide solution described in step S5 is 8%-12%.
Further, the rotating speed of centrifuge described in step S7 is 3500-6000r/min.
Further, described in step S7, the mesh number of sieve is 300-600 mesh.
The method have the advantages that
(1) present invention adds the Fe that acid corrosion equipment can be produced by reducing agent3+It is reduced to the Fe of light color2+, Avoid Fe3+The whiteness of the Color influences active hargil brought;
(2) the load hydrogen sodium oxide activated clay production efficiency of the present invention is high, energy consumption and low cost;
(3) the load hydrogen sodium oxide active hargil alkali capacity that the present invention produces is 19-19.4mmol/g, and whiteness is high And it is stable;
(4) present invention uses centrifuging to remove water, and efficiency is high so that whole production technology cycle time;
(5) the recyclable recycling of gained spent acid of the present invention, effectively reduces acid and processes the cost of sewage, favorably In energy-saving and emission-reduction.
[detailed description of the invention]
For ease of being more fully understood that the present invention, being illustrated by following example, these embodiments belong to this Bright protection domain, but it is not intended to protection scope of the present invention.
The preparation method of a kind of load hydrogen sodium oxide active hargil, comprises the following steps:
S1: by bentonite and active hargil waste water that concentration is 13%-16% by weight for 1.6-2.2:10-14 Mixing, stirs under the conditions of rotating speed is 200-500r/min, prepares pasty material A;
S2: the pasty material A that step S1 prepares is joined in the inorganic mixed acid that concentration is 11%-20%, Described inorganic mixed acid is the sulphuric acid of concentration 16-18wt%, the carbonic acid of concentration 32-36wt%, concentration 18-20wt% The mixed acid of oxalic acid 2-6:3-5:2-3 by volume composition, the weight ratio of pasty material A and inorganic mixed acid For 1-3.2:4-16, under the conditions of rotating speed is 200-550r/min, add ammonium sulfide stirring, ammonium sulfide and slurry The weight ratio of material A is 1-2:50-150, is heated to 82-93 DEG C, reacts 1.2-3.2h under the conditions of being maintained at 82-93 DEG C, Prepare pasty material B;
S3: the pasty material B that step S2 prepares is carried out filter pressing under the conditions of pressure is 0.9-0.95MPa, Prepared moisture content is the filter cake A of 32%-45%;
S4: the filter cake A prepared to step S3 adds water stirring and dissolving, and amount of water is the 6-7.5 of filter cake A weight Times, stirring and dissolving filter cake A adds flocculant stirring 0.4-1.2h after completing makes solution precipitate, by precipitate in pressure Power is to carry out filter pressing under the conditions of 0.9-0.95MPa, and prepared moisture content is the filter cake B of 32%-45%, described flocculation Agent includes that the one in organic flocculant and inorganic flocculating agent, described organic flocculant include sodium polyacrylate, gather One in calcium acrylate, acrylamide, described inorganic flocculating agent includes in bodied ferric sulfate, polyaluminium sulfate One;
S5: add water stirring and dissolving by the filter cake B that step S4 prepares, and amount of water is the 5-6.5 of filter cake B weight Times, after stirring and dissolving filter cake B completes, adding concentration is the sodium hydroxide solution of 8%-12%;
S6: the slurry material C that step S5 prepares is carried out filter pressing under the conditions of pressure is 0.9-0.95MPa, system Obtain the filter cake C that moisture content is 32%-45%;
S7: the filter cake C that step S6 prepares is placed in centrifuge, is 3500-6000r/min at centrifugal rotational speed Under the conditions of remove water to and pulverize after filter cake C moisture content≤5%, gained ground product crosses 300-600 mesh sieve, prepares negative Carry sodium hydroxide active hargil.
Below by more specifically embodiment, the present invention will be described.
Embodiment 1
The preparation method of a kind of load hydrogen sodium oxide active hargil, comprises the following steps:
S1: bentonite and the active hargil waste water that concentration is 15% are mixed by weight for 2:12, at rotating speed For stirring under the conditions of 400r/min, prepare pasty material A;
S2: the pasty material A that step S1 prepares is joined in the inorganic mixed acid that concentration is 15%, described Inorganic mixed acid be the sulphuric acid of concentration 17wt%, the carbonic acid of concentration 34wt%, concentration 19wt% oxalic acid by body The long-pending mixed acid than 4:3:2 composition, pasty material A is 2:10 with the weight ratio of inorganic mixed acid, at rotating speed is Adding ammonium sulfide stirring under the conditions of 400r/min, ammonium sulfide is 2:120 with the weight ratio of pasty material A, heating To 85 DEG C, react 2.5h under the conditions of being maintained at 85 DEG C, prepare pasty material B;
S3: the pasty material B that step S2 prepares is carried out under the conditions of pressure is 0.92MPa filter pressing, prepares Moisture content is the filter cake A of 40%;
S4: the filter cake A prepared to step S3 adds water stirring and dissolving, and amount of water is 7 times of filter cake A weight, Stirring and dissolving filter cake A adds sodium polyacrylate after completing and polyaluminium sulfate stirring 0.9h makes solution precipitate, will Precipitate carries out filter pressing under the conditions of pressure is 0.92MPa, and prepared moisture content is the filter cake B of 38%;
S5: add water stirring and dissolving by the filter cake B that step S4 prepares, and amount of water is 6 times of filter cake B weight, After stirring and dissolving filter cake B completes, adding concentration is the sodium hydroxide solution of 10%, prepares slurry material C;
S6: the slurry material C that step S5 prepares is carried out under the conditions of pressure is 0.92MPa filter pressing, prepares and contains Water rate is the filter cake C of 39%;
S7: the filter cake C that step S6 prepares is placed in centrifuge, is 5000r/min condition at centrifugal rotational speed Under to remove water to filter cake C moisture content be to pulverize after 4%, gained ground product crosses 500 mesh sieves, prepares load hydrogen oxidation Sodium active hargil.
Embodiment 2
The preparation method of a kind of load hydrogen sodium oxide active hargil, comprises the following steps:
S1: bentonite and the active hargil waste water that concentration is 16% are mixed by weight for 2.2:14, is turning Speed, for stirring under the conditions of 500r/min, prepares pasty material A;
S2: the pasty material A that step S1 prepares is joined in the inorganic mixed acid that concentration is 20%, described Inorganic mixed acid be the sulphuric acid of concentration 18wt%, the carbonic acid of concentration 36wt%, concentration 20wt% oxalic acid by body The long-pending mixed acid than 6:5:3 composition, pasty material A is 3.2:16 with the weight ratio of inorganic mixed acid, at rotating speed For adding ammonium sulfide stirring under the conditions of 550r/min, ammonium sulfide is 2:150 with the weight ratio of pasty material A, adds Heat, to 93 DEG C, is reacted 1.2h, is prepared pasty material B under the conditions of being maintained at 93 DEG C;
S3: the pasty material B that step S2 prepares is carried out under the conditions of pressure is 0.95MPa filter pressing, prepares Moisture content is the filter cake A of 45%;
S4: the filter cake A prepared to step S3 adds water stirring and dissolving, and amount of water is 7.5 times of filter cake A weight, Stirring and dissolving filter cake A adds bodied ferric sulfate stirring 1.2h after completing makes solution precipitate, by precipitate at pressure For carrying out filter pressing under the conditions of 0.95MPa, prepared moisture content is the filter cake B of 45%;
S5: add water stirring and dissolving by the filter cake B that step S4 prepares, and amount of water is 6.5 times of filter cake B weight, After stirring and dissolving filter cake B completes, adding concentration is the sodium hydroxide solution of 12%, prepares slurry material C;
S6: the slurry material C that step S5 prepares is carried out under the conditions of pressure is 0.95MPa filter pressing, prepares and contains Water rate is the filter cake C of 45%;
S7: the filter cake C that step S6 prepares is placed in centrifuge, is 6000r/min condition at centrifugal rotational speed Under to remove water to filter cake C moisture content be to pulverize after 5%, gained ground product crosses 600 mesh sieves, prepares load hydrogen oxidation Sodium active hargil.
Embodiment 3
The preparation method of a kind of load hydrogen sodium oxide active hargil, comprises the following steps:
S1: bentonite and the active hargil waste water that concentration is 13% are mixed by weight for 1.6:10, is turning Speed, for stirring under the conditions of 200r/min, prepares pasty material A;
S2: the pasty material A that step S1 prepares is joined in the inorganic mixed acid that concentration is 11%, described Inorganic mixed acid be the sulphuric acid of concentration 16wt%, the carbonic acid of concentration 32wt%, concentration 18wt% oxalic acid by body The long-pending mixed acid than 2:3:2 composition, pasty material A is 1:4 with the weight ratio of inorganic mixed acid, at rotating speed is Adding ammonium sulfide stirring under the conditions of 200r/min, ammonium sulfide is 1:50 with the weight ratio of pasty material A, heating To 82 DEG C, react 3.2h under the conditions of being maintained at 82 DEG C, prepare pasty material B;
S3: the pasty material B that step S2 prepares is carried out under the conditions of pressure is 0.9MPa filter pressing, prepares Moisture content is the filter cake A of 32%;
S4: the filter cake A prepared to step S3 adds water stirring and dissolving, and amount of water is 6 times of filter cake A weight, Stirring and dissolving filter cake A adds acrylamide stirring 0.4h after completing makes solution precipitate, and by precipitate at pressure is Carrying out filter pressing under the conditions of 0.9MPa, prepared moisture content is the filter cake B of 32%;
S5: add water stirring and dissolving by the filter cake B that step S4 prepares, and amount of water is 5 times of filter cake B weight, After stirring and dissolving filter cake B completes, adding concentration is the sodium hydroxide solution of 8%, prepares slurry material C;
S6: the slurry material C that step S5 prepares is carried out under the conditions of pressure is 0.9MPa filter pressing, prepares and contains Water rate is the filter cake C of 32%;
S7: the filter cake C that step S6 prepares is placed in centrifuge, is 3500r/min condition at centrifugal rotational speed Under to remove water to filter cake C moisture content be to pulverize after 4%, gained ground product crosses 300 mesh sieves, prepares load hydrogen oxidation Sodium active hargil.
In embodiment, load hydrogen sodium oxide active hargil moisture content, alkali solubility, alkali volumetric analysis result see table.
As seen from the above table, load hydrogen sodium oxide active hargil product moisture content≤5% prepared by the present invention, alkali is molten Xie Du is 0.51-0.52gNaOH/100mlH2O, alkali capacity is 19-19.4mmol/g, it can be seen that, this The load hydrogen sodium oxide active hargil quality that bright technique produces is high and stable.
Above content it cannot be assumed that the present invention be embodied as be confined to these explanation, for skill belonging to the present invention For the those of ordinary skill in art field, without departing from the inventive concept of the premise, it is also possible to make some letters Single deduction or replace, all should be considered as belonging to the patent protection model that the present invention is determined by the claims submitted to Enclose.

Claims (7)

1. the preparation method of a load hydrogen sodium oxide active hargil, it is characterised in that: comprise the following steps:
S1: by bentonite and active hargil waste water that concentration is 13%-16% by weight for 1.6-2.2:10-14 Mixing, stirs under the conditions of rotating speed is 200-500r/min, prepares pasty material A;
S2: the pasty material A that step S1 prepares is joined in the inorganic mixed acid that concentration is 11%-20%, Described inorganic mixed acid is the sulphuric acid of concentration 16-18wt%, the carbonic acid of concentration 32-36wt%, concentration 18-20wt% The mixed acid of oxalic acid 2-6:3-5:2-3 by volume composition, the weight ratio of pasty material A and inorganic mixed acid For 1-3.2:4-16, under the conditions of rotating speed is 200-550r/min, add ammonium sulfide stirring, ammonium sulfide and slurry The weight ratio of material A is 1-2:50-150, is heated to 82-93 DEG C, reacts 1.2-3.2h under the conditions of being maintained at 82-93 DEG C, Prepare pasty material B;
S3: the pasty material B that step S2 prepares is carried out filter pressing under the conditions of pressure is 0.9-0.95MPa, Prepared moisture content is the filter cake A of 32%-45%;
S4: the filter cake A prepared to step S3 adds water stirring and dissolving, and amount of water is the 6-7.5 of filter cake A weight Times, stirring and dissolving filter cake A adds flocculant stirring 0.4-1.2h after completing makes solution precipitate, by precipitate in pressure Power is to carry out filter pressing under the conditions of 0.9-0.95MPa, and prepared moisture content is the filter cake B of 32%-45%;
S5: add water stirring and dissolving by the filter cake B that step S4 prepares, and amount of water is the 5-6.5 of filter cake B weight Times, after stirring and dissolving filter cake B completes, add sodium hydroxide solution, prepare slurry material C;
S6: the slurry material C that step S5 prepares is carried out filter pressing under the conditions of pressure is 0.9-0.95MPa, system Obtain the filter cake C that moisture content is 32%-45%;
S7: the filter cake C that step S6 prepares is placed in centrifuge and removes water to powder after filter cake C moisture content≤5% Broken, gained ground product sieves, and prepares load hydrogen sodium oxide active hargil.
The preparation method of load hydrogen sodium oxide active hargil the most according to claim 1, it is characterised in that Flocculant described in step S4 includes the one in organic flocculant and inorganic flocculating agent.
The preparation method of load hydrogen sodium oxide active hargil the most according to claim 3, it is characterised in that Described organic flocculant includes the one in sodium polyacrylate, calcium polyacrylate (CPA), acrylamide.
The preparation method of load hydrogen sodium oxide active hargil the most according to claim 3, it is characterised in that Described inorganic flocculating agent includes one or more in bodied ferric sulfate, polyaluminium sulfate.
The preparation method of load hydrogen sodium oxide active hargil the most according to claim 1, it is characterised in that Concentration of sodium hydroxide solution described in step S5 is 8%-12%.
The preparation method of load hydrogen sodium oxide active hargil the most according to claim 1, it is characterised in that The rotating speed of centrifuge described in step S7 is 3500-6000r/min.
The preparation method of load hydrogen sodium oxide active hargil the most according to claim 1, it is characterised in that Described in step S7, the mesh number of sieve is 300-600 mesh.
CN201610260163.2A 2016-04-25 2016-04-25 Preparation method of activated clay loaded sodium hydroxide Pending CN105948069A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109954477A (en) * 2017-12-26 2019-07-02 金昌红泉膨润土有限责任公司 A kind of atlapulgite acid lowering agent

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102557057A (en) * 2011-12-28 2012-07-11 攀枝花学院 Active argil and preparation method thereof
CN105271277A (en) * 2015-02-15 2016-01-27 广西隆安瑞丰工贸有限公司 Preparation method for calcium hydrate loading activated clay
CN105293797A (en) * 2015-02-15 2016-02-03 广西隆安瑞丰工贸有限公司 Method for co-production of aluminum potassium sulfate and gypsum through activated clay production mother liquid

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102557057A (en) * 2011-12-28 2012-07-11 攀枝花学院 Active argil and preparation method thereof
CN105271277A (en) * 2015-02-15 2016-01-27 广西隆安瑞丰工贸有限公司 Preparation method for calcium hydrate loading activated clay
CN105293797A (en) * 2015-02-15 2016-02-03 广西隆安瑞丰工贸有限公司 Method for co-production of aluminum potassium sulfate and gypsum through activated clay production mother liquid

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109954477A (en) * 2017-12-26 2019-07-02 金昌红泉膨润土有限责任公司 A kind of atlapulgite acid lowering agent

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Application publication date: 20160921