CN111099618A - Process for preparing mordenite - Google Patents
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- CN111099618A CN111099618A CN201811260636.4A CN201811260636A CN111099618A CN 111099618 A CN111099618 A CN 111099618A CN 201811260636 A CN201811260636 A CN 201811260636A CN 111099618 A CN111099618 A CN 111099618A
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- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/26—Mordenite type
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Abstract
The invention relates to the field of catalysts, and discloses a preparation method of mordenite, which comprises the following steps: 1) carrying out a first contact reaction on silicon-containing wastewater and one or more selected from acid solution, alkali solution and silica sol to ensure that the pH of the obtained solution is 5-10, and carrying out first solid-liquid separation on a product after the first contact reaction; 2) and carrying out a second contact reaction on the solid phase obtained by the first separation, an aluminum source, a silicon source and an alkali source, and sequentially carrying out crystallization, second solid-liquid separation and cleaning on a product obtained after the second contact reaction. The method has the advantages of high silicon recovery rate and good safety.
Description
Technical Field
The invention relates to the field of catalysts, in particular to a preparation method of mordenite.
Background
The synthesized mordenite has the structural characteristics of high specific surface area, high water stability, high thermal stability, uniform pore size and the like, is widely used as a catalytic reaction material, an ion exchange material and an adsorption separation material, and has wide application in the field of chemical oil refining. In general, in the preparation process of mordenite, after the crystallization process is completed, the crystallized product needs to be filtered and cleaned to remove soluble silicon and aluminum remained on the inner and outer surfaces of the mordenite, so that silicon-containing wastewater can be generated. The wastewater has high suspended matter content and can not be directly discharged.
Patent US4164551 discloses a method for utilizing NaY molecular sieve synthesis mother liquor. The method is characterized in that mother liquor obtained after the NaY molecular sieve is synthesized for many times by a conventional gel method is collected, acidic aluminum salt is added, the pH value of a system is adjusted to 6-7, intermediate silica-alumina gel is formed, and a filter cake is obtained by filtering and used for the next synthesis of the NaY molecular sieve. According to the method, silicate radicals in the mother liquor are synthesized by using the NaY molecular sieve, sodium sulfate in the mother liquor is separated from a filter cake, and the silica-alumina gel can be used for subsequent synthesis of the NaY molecular sieve, so that the reuse ratio of the silica-alumina gel is increased to 45%, the utilization rate of silicon is increased to more than 90%, but a method for treating silicon-containing wastewater generated in the subsequent preparation process is not involved.
The utilization of NaY crystallization mother liquor is described in the literature (Industrial catalysis, 10 (2002): 56-60). The method is characterized in that in the process of synthesizing the Y-shaped molecular sieve by a guide agent method, mother liquor is separated, a certain amount of aluminum sulfate solution is added into the mother liquor to precipitate silicon, and qualified silica-alumina gel can be obtained after filtration and washing for recycling. The method obviously reduces the treatment load of the silicon-containing sewage and improves the qualification rate of the discharged sewage suspended matters, but does not relate to a treatment method of the silicon-containing sewage generated in the subsequent preparation process.
Chinese patent CN1111508C discloses a method for synthesizing mordenite by using Beta zeolite synthesis mother liquor. The method is characterized in that original synthetic mother liquor of Beta zeolite is used as a medium, a silicon source, an aluminum source, fluoride and optional sulfuric acid are added into the medium, and the high-silicon mordenite is obtained through crystallization, filtration, cleaning and drying. However, the present invention does not reuse the mordenite synthesis mother liquor.
Disclosure of Invention
The invention aims to solve the problems of low silicon recovery rate and environmental pollution caused by wastewater in the mordenite preparation method in the prior art, and provides a clean preparation method of mordenite, which has the advantages of high silicon recovery rate and good safety.
In order to achieve the above object, the present invention provides a method for preparing mordenite, which comprises the steps of:
1) carrying out a first contact reaction on silicon-containing wastewater and one or more selected from acid solution, alkali solution and silica sol to ensure that the pH of the obtained solution is 5-10, and carrying out first solid-liquid separation on a product after the first contact reaction;
2) and carrying out a second contact reaction on the solid phase obtained by the first separation, an aluminum source, a silicon source and an alkali source, and sequentially carrying out crystallization, second solid-liquid separation and cleaning on a product obtained after the second contact reaction.
Preferably, the silicon-containing wastewater is wastewater generated in the preparation of mordenite.
Preferably, the silicon-containing wastewater is mother liquor obtained by the second solid-liquid separation and/or cleaning liquid obtained by cleaning.
Preferably, the content of silicon element in the silicon-containing wastewater is 10-20000 mg/L; more preferably, the content of the silicon element in the silicon-containing wastewater is 150-16000 mg/L.
Preferably, the pH of the silicon-containing wastewater is 8-14.
Preferably, the conditions of the contact reaction include: the contact temperature is 70-99 ℃, and the contact time is 4-12 h.
Preferably, the concentration of the acid solution is 30 to 40 wt%, the concentration of the alkali solution is 30 to 50 wt%, and the concentration of the silica sol is 1 to 40 wt%.
Preferably, the alkali solution is a solution of sodium hydroxide and/or potassium hydroxide.
Preferably, the acid solution is one or more of nitric acid, sulfuric acid and hydrochloric acid.
Preferably, the method further comprises: the colloid-containing mixed liquor is aged before the first solid-liquid separation.
Preferably, the aging conditions include: the aging temperature is 20-99 ℃, and the aging time is 5-10 hours.
Preferably, the first solid-liquid separation is performed so that the solid content in the solid phase obtained by the first solid-liquid separation is 15% by weight or more.
Preferably, the first solid-liquid separation is carried out at 70 to 99 ℃.
Preferably, the aluminum source is one or more of sodium aluminate, aluminum sulfate, aluminum nitrate, aluminum chloride, aluminum sol and pseudo-boehmite.
Preferably, the silicon source is one or more of water glass, white carbon black, silica sol and silica gel.
Preferably, the alkali source is one or more of sodium hydroxide, potassium hydroxide and ammonia water.
Preferably, the crystallization conditions include: the crystallization temperature is 120-220 ℃, and the crystallization time is 1-4 days.
Preferably, the washing is performed using an aqueous acid solution. More preferably, the acid is one or more of sulfuric acid, hydrochloric acid, hydrofluoric acid and citric acid.
Through the technical scheme, silicon in the silicon-containing wastewater obtained in the solid-liquid separation and cleaning processes is separated and recovered and is used as a silicon source for preparing the mordenite, so that the utilization rate of silicon is improved, the resource recycling is realized, and the waste amount generated in the production process of the mordenite is reduced. The method for treating the silicon-containing wastewater generated in the mordenite production process is simple and convenient in recovery mode, can effectively realize the reutilization of recoverable resources in the silicon-containing wastewater without special treatment, and obtains better technical effect.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a preparation method of mordenite, which comprises the following steps:
1) carrying out a first contact reaction on silicon-containing wastewater and one or more selected from acid solution, alkali solution and silica sol to ensure that the pH of the obtained solution is 5-10, and carrying out first solid-liquid separation on a product after the first contact reaction;
2) and carrying out a second contact reaction on the solid phase obtained by the first separation, an aluminum source, a silicon source and an alkali source, and sequentially carrying out crystallization, second solid-liquid separation and cleaning on a product obtained after the second contact reaction.
In the method for preparing mordenite of the present invention, the silicon-containing wastewater is not particularly limited. For example, the content of silicon element in the silicon-containing wastewater can be 10-20000 mg/L; preferably, the content of the silicon element in the silicon-containing wastewater is 150-16000 mg/L. For example, the pH of the silicon-containing wastewater may be 8 to 14. By setting the silicon element content and the pH in the silicon-containing wastewater within the above content ranges, elements such as silicon and aluminum in the silicon-containing wastewater can be utilized more sufficiently.
According to the present invention, the silicon-containing wastewater may be wastewater produced in the preparation of mordenite. Preferably, the silicon-containing wastewater is mother liquor obtained by the second solid-liquid separation and/or cleaning liquid obtained by cleaning. Wherein, when the mother liquor obtained by the second solid-liquid separation is used as the silicon-containing wastewater, the first contact reaction is preferably carried out by using alkali solution and/or silica sol; when the cleaning liquid obtained by cleaning is used, the first contact reaction is preferably carried out using an acid solution.
In the invention, the mother liquor obtained by the second solid-liquid separation and/or the cleaning solution obtained by cleaning are/is recovered as silicon-containing wastewater, so that the silicon and aluminum contents in the mordenite preparation wastewater can be reduced, the utilization rate of raw materials is improved, the wastewater treatment cost is reduced, and the pollution is reduced. The solid phase obtained by the first separation is used as a silicon source and/or an aluminum source in the preparation of the mordenite, so that the amount of the silicon source and the aluminum source required in the preparation of the mordenite is reduced, and the preparation cost is reduced.
As the acid solution used in the present invention, one or more of nitric acid, sulfuric acid, and hydrochloric acid is preferable.
As the alkali solution used in the present invention, a solution of sodium hydroxide and/or potassium hydroxide is preferable.
As the silica sol used in the present invention, silica particles are preferably in the range of 1 to 40nm, more preferably 5 to 30 nm.
In order to recover elements such as silicon and aluminum in the silicon-containing wastewater better, the concentration of the acid solution is preferably 30-40 wt%, the concentration of the alkali solution is preferably 30-50 wt%, and the concentration of the silica sol is preferably 1-40 wt%; more preferably, the concentration of the acid solution is 35 to 40 wt%, the concentration of the alkali solution is 35 to 45 wt%, and the concentration of the silica sol is 20 to 35 wt%.
In order that elements such as silicon and aluminum in the silicon-containing wastewater can be sufficiently reacted with one or more selected from the group consisting of an acid solution, an alkali solution and a silica sol in the first contact reaction process, preferably, the conditions of the first contact reaction include: the contact temperature is 70-99 ℃, and the contact time is 4-12 h; more preferably, the contact temperature is 80-98 ℃ and the contact time is 5-8 h. By carrying out the first contact reaction under the above conditions, elements such as silicon and aluminum can be separated as much as possible, thereby facilitating subsequent recovery.
The "first contact reaction and making the pH of the resulting solution 5 to 10" in the present invention means that the pH of the resulting solution after the completion of the first contact reaction is 5 to 10. From the viewpoint of improving the recovery efficiency of the elements and the crystallinity of the mordenite to be produced, the above pH may preferably be 7 to 9.
The first solid-liquid separation method may be, for example, filtration, sedimentation, centrifugation or the like, and filtration using a belt filter is more preferable. According to a preferred embodiment of the present invention, the solid content in the solid phase obtained by the first solid-liquid separation is 15% by weight or more, preferably 17% by weight or more, and more preferably 20% by weight or more.
In addition, in order to stabilize the mixed liquid obtained by the first contact reaction or aging and to improve the recovery rate of the elements, it is preferable that the first solid-liquid separation is performed at 70 to 99 ℃.
In the method for producing mordenite of the present invention, the aluminum source, the silicon source and the alkali source are not particularly limited, and the method can be carried out using various conventional aluminum sources, silicon sources and alkali sources which can be used for the production of mordenite. As the aluminum source, one or more of sodium aluminate, aluminum sulfate, aluminum nitrate, aluminum chloride, aluminum sol, and pseudo-boehmite; examples of the silicon source include one or more of water glass, white carbon, silica sol, and silica gel; the alkali source may be one or more of sodium hydroxide, potassium hydroxide and aqueous ammonia. Among them, aluminum sol is preferably used as the aluminum source, and the concentration thereof may be 5 to 20% by weight.
In order to ensure the quality of the obtained mordenite, the weight ratio of the solid phase obtained by the first separation to the silicon source is 1: 50 or more, preferably 1: 8-40.
According to a preferred embodiment of the present invention, in order to further improve the element recycling rate, the method further comprises: the colloid-containing mixed liquor is aged before the first solid-liquid separation. Preferably, the aging conditions include: the aging temperature is 20-99 ℃, and the aging time is 5-10 hours; more preferably, the aging temperature is 35-95 ℃ and the aging time is 8-10 hours.
In the method for preparing mordenite of the present invention, the manner of performing the second contact reaction, the crystallization, the second solid-liquid separation, and the washing is not particularly limited, and any conventional method that can be used for preparing mordenite can be used, and the purpose of preparing mordenite can be achieved.
The second solid-liquid separation method may be, for example, filtration, centrifugation or the like, and among them, suction filtration or centrifugation is preferable.
As the conditions for crystallization, there may be included: the crystallization temperature is 120-220 ℃, the crystallization time is 1-4 days, preferably, the crystallization temperature is 140-180 ℃, and the crystallization time is 2-4 days. The crystallization can be carried out, for example, in a stainless steel reactor.
As the washing, an aqueous solution of an acid may be used. Preferably, the acid is one or more of sulfuric acid, hydrochloric acid, hydrofluoric acid and citric acid. The concentration of the cleaning liquid used for the cleaning may be, for example, 0.01 to 0.15 g/mL. The number of washing may be 2 or more, preferably 3 to 5.
The present invention will be described in detail below by way of examples. In the following examples, the relative crystallinity of mordenite was determined by taking a sample of known crystallinity as a standard, adding the intensity values of the eight characteristic peaks in the XRD pattern of the test sample and dividing by the intensity value of the standard. The molecular sieve product yield is obtained by sampling the mordenite molecular sieve finished product, roasting the mordenite molecular sieve finished product in a muffle furnace at 500 ℃ for 2 hours to obtain the dry basis weight of the finished product, and then dividing the dry basis weight by the total weight of silicon and aluminum in the feed by silicon oxide and aluminum oxide. The recovery rate of silicon element in the silicon-containing wastewater adopts a detection method provided by the industry standard HG-T2521-2008 industrial silica sol to respectively detect the content X of silicon dioxide in the wastewater before and after solid-liquid separation0、X1By the formula:
thus obtaining the product.
Comparative example 1
Using silica sol (30 wt%, 1600kg) as a silicon source, alumina sol (160kg15 wt%) as an aluminum source, sodium hydroxide solution (50 wt%, 90L) as an alkali source to perform a contact reaction, and sequentially crystallizing (160 ℃, 4 days), performing a first solid-liquid separation (centrifugation), and washing (using 0.03g/mL citric acid aqueous solution, washing 2 times); the mordenite is obtained, and the physical property analysis parameters are shown in the table 1.
Example 1
The silicon-containing wastewater treated in this example was the mother liquor and the wash filtrate produced in the second solid-liquid separation process in the production of mordenite of comparative example 1.
The following process flow is adopted in the embodiment to treat the silicon-containing wastewater.
(1) Adding a sodium hydroxide solution (with the mass concentration of 32%) into the silicon-containing wastewater, wherein the contact temperature is 95 ℃, the contact time is 5 hours, the pH value of the silicon-containing wastewater after the contact reaction is finished is 8, and then aging the silicon-containing wastewater for 5 hours under the condition of stirring at 90 ℃ to obtain a mixture of silicon-containing colloids.
(2) The mixture of the silicon-containing colloids obtained in step (1) was filtered by a horizontal tape filter to obtain a silicon-containing cake (containing 74% by weight of water), and the recovery rate of elemental silicon is shown in Table 1.
(3) The recovered siliceous filter cake was used as a silicon source while a part of fresh silicon source was replenished (the weight ratio of the siliceous filter cake to the fresh silicon source was 1: 40), and mordenite was produced under the remaining conditions in the manner of comparative example 1, and the physical property analysis parameters thereof are shown in table 1.
(4) And (4) repeating the steps (1) to (3), and recycling the silicon-containing wastewater to be used as a production raw material of the next batch of mordenite.
Example 2
Mordenite was produced under the conditions and procedures described in example 1 except that in step (1), silica sol (15nm, 30 wt%) was used instead of sodium hydroxide solution and aged at 90 ℃ for 5 hours with stirring, and the recovery of silicon element and analytical parameters for the physical properties of the mordenite produced from the siliceous filter cake obtained in step (2) are shown in Table 1.
TABLE 1
| Serial number | Relative degree of crystallinity% | The product yield is% | Recovery rate of silicon element |
| Comparative example 1 | 88 | 93 | / |
| Example 1 | 89 | 92 | 96 |
| Example 2 | 90 | 94 | 95 |
From table 1 it can be seen that the crystallinity of the mordenite and the yield of the molecular sieve of example 1 and example 2 are substantially the same as in comparative example 1, indicating that the quality of the mordenite produced by the process of the present invention is at the same level as in comparative example 1.
Examples 3 to 5
Mordenite was produced under the conditions and procedures described in example 1 except that the pH of the siliceous wastewater after completion of the contact reaction in step (1) was changed to 7, 9 and 10, respectively, to obtain a siliceous filter cake. The recovery rates of silicon element were 93 wt%, 94 wt% and 92 wt%, respectively. The relative crystallinity of the mordenite obtained was 87%, 88% and 89%, respectively, and the product yields were 93%, 90% and 92%, respectively.
Examples 6 to 8
Mordenite was produced under the conditions and by the procedure described in example 1 except that the contact temperature of sodium hydroxide with the silicon-containing wastewater in step (1) was changed to 80 deg.C, 88 deg.C and 98 deg.C, respectively, to obtain a silicon-containing cake. The elemental silicon recovery rates were 92 wt%, 94 wt%, and 96 wt%, respectively. The relative crystallinity of the mordenite obtained was 85%, 87% and 89%, respectively, and the product yields were 86%, 90% and 92%, respectively.
Examples 9 to 11
Mordenite was produced under the conditions and procedures described in example 1 except that the contact time of the sodium hydroxide solution with the siliceous waste water in step (1) was changed to 4 hours, 8 hours and 12 hours, respectively, to obtain a siliceous filter cake. The recovery rates of silicon element were 91 wt%, 96 wt%, and 94 wt%, respectively. The relative crystallinity of the mordenite obtained was 85%, 89% and 89%, respectively, and the product yields were 87%, 92% and 90%, respectively.
Examples 12 to 14
Mordenite was produced under the conditions and procedures described in example 1 except that the ageing time in step (1) was changed to 6 hours, 8 hours and 10 hours respectively to obtain a siliceous filter cake. The recovery rates of silicon element were 91 wt%, 93 wt%, and 96 wt%, respectively. The relative crystallinity of the mordenite obtained was 89%, 90% and 89%, respectively, and the product yields were 85%, 89% and 92%, respectively.
Examples 15 to 17
Mordenite was produced under the conditions and procedures described in example 1 except that the ageing temperature in step (1) was changed to 35 deg.C, 65 deg.C and 95 deg.C respectively to obtain a siliceous filter cake. The recovery rates of silicon element were 90 wt%, 92 wt%, and 96 wt%, in this order. The relative crystallinity of the mordenite obtained was 88%, 90% and 89%, respectively, and the product yields were 84%, 87% and 92%, respectively.
Examples 18 to 20
Mordenite was produced under the conditions and procedures described in example 2 except that the pH of the siliceous wastewater after completion of the contact reaction in step (1) was changed to 6, 7 and 9, respectively, to obtain a siliceous filter cake. The recovery rates of silicon element were 92 wt%, 95 wt% and 95 wt%, respectively. The relative crystallinity of the mordenite obtained was 88%, 89% and 90%, respectively, and the product yields were 90%, 92% and 94%, respectively.
Examples 21 to 23
Mordenite was produced under the conditions and by the procedure described in example 2 except that the contact temperature of the silica sol with the siliceous waste water in step (1) was changed to 80 deg.C, 88 deg.C and 98 deg.C, respectively, to obtain a siliceous filter cake. The recovery rates of silicon element were 93 wt%, 94 wt% and 95 wt%, respectively. The relative crystallinity of the mordenite obtained was 84%, 88% and 90%, respectively, and the product yields were 88%, 91% and 94%, respectively.
Examples 24 to 26
Mordenite was produced under the conditions and procedures described in example 2 except that the contact time of the silica sol with the siliceous waste water in step (1) was changed to 4 hours, 8 hours and 12 hours, respectively, to obtain a siliceous filter cake. The recovery rates of silicon element were 90 wt%, 95 wt%, and 93 wt%, respectively. The relative crystallinity of the mordenite obtained was 86%, 90% and 90%, respectively, and the product yields were 88%, 94% and 92%, respectively.
Examples 27 to 29
Mordenite was produced under the conditions and procedures described in example 2 except that the ageing time in step (1) was changed to 6 hours, 8 hours and 10 hours respectively to obtain a siliceous filter cake. The recovery rates of silicon element were 92 wt%, 94 wt% and 95 wt%, respectively. The relative crystallinity of the mordenite obtained was 88%, 90% and 90%, respectively, and the product yields were 83%, 93% and 94%, respectively.
Examples 30 to 32
Mordenite was produced under the conditions and procedures described in example 2 except that the ageing temperature in step (1) was changed to 35 deg.C, 65 deg.C and 95 deg.C respectively to obtain a siliceous filter cake. The recovery rates of silicon element were 92 wt%, 94 wt% and 95 wt%, respectively. The relative crystallinity of the mordenite obtained was 87%, 90% and 92% respectively, and the product yields were 86%, 90% and 94% respectively.
By comparing the crystallinity and yield of the mordenite in examples 1 to 32 and comparative example 1 above, it can be seen that the process of the present invention produces a mordenite of the same quality as that produced in comparative example 1.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for preparing mordenite, which is characterized by comprising the following steps:
1) carrying out a first contact reaction on silicon-containing wastewater and one or more selected from acid solution, alkali solution and silica sol to ensure that the pH of the obtained solution is 5-10, and carrying out first solid-liquid separation on a product after the first contact reaction;
2) and carrying out a second contact reaction on the solid phase obtained by the first separation, an aluminum source, a silicon source and an alkali source, and sequentially carrying out crystallization, second solid-liquid separation and cleaning on a product obtained after the second contact reaction.
2. The process of claim 1, wherein the siliceous wastewater is a wastewater produced in the manufacture of mordenite;
preferably, the silicon-containing wastewater is mother liquor obtained by second solid-liquid separation and/or cleaning solution obtained by cleaning;
preferably, the content of silicon element in the silicon-containing wastewater is 10-20000 mg/L;
preferably, the content of the silicon element in the silicon-containing wastewater is 150-16000 mg/L.
3. The method according to claim 1, wherein the pH of the silicon-containing wastewater is 8 to 14.
4. The method of claim 1, wherein the conditions of the first contact reaction comprise: the contact temperature is 70-99 ℃, and the contact time is 4-12 h.
5. The method according to any one of claims 1 to 4, wherein the concentration of the acid solution is 30 to 40 wt.%, the concentration of the alkali solution is 30 to 50 wt.%, and the concentration of the silica sol is 1 to 40 wt.%;
preferably, the alkali solution is a solution of sodium hydroxide and/or potassium hydroxide;
preferably, the acid solution is one or more of nitric acid, sulfuric acid and hydrochloric acid.
6. The method of any of claims 1-4, wherein the method further comprises: before the first solid-liquid separation, the mixed liquid containing the colloid is aged;
preferably, the aging conditions include: the aging temperature is 20-99 ℃, and the aging time is 5-10 hours.
7. The process according to any one of claims 1 to 4, wherein the first solid-liquid separation is carried out so that the solid content in the solid phase obtained by the first solid-liquid separation is 15% by weight or more;
preferably, the first solid-liquid separation is carried out at 70 to 99 ℃.
8. The process of any one of claims 1-4, wherein the aluminum source is one or more of sodium aluminate, aluminum sulfate, aluminum nitrate, aluminum chloride, aluminum sol, and pseudo-boehmite;
preferably, the silicon source is one or more of water glass, white carbon black, silica sol and silica gel;
preferably, the alkali source is one or more of sodium hydroxide, potassium hydroxide and ammonia water.
9. The method of any of claims 1-4, wherein the crystallization conditions comprise: the crystallization temperature is 120-220 ℃, and the crystallization time is 1-4 days.
10. The method according to any one of claims 1 to 4, wherein the washing is performed using an aqueous solution of an acid;
preferably, the acid is one or more of sulfuric acid, hydrochloric acid, hydrofluoric acid and citric acid.
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| CN105540943A (en) * | 2015-10-30 | 2016-05-04 | 中国石油化工股份有限公司 | Silicon-containing wastewater treatment method, silicon-containing wastewater utilization system, molecular sieve preparation method and molecular sieve preparation system |
| CN106542543A (en) * | 2016-10-17 | 2017-03-29 | 中国石油化工股份有限公司 | The clean preparation method of modenite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105540943A (en) * | 2015-10-30 | 2016-05-04 | 中国石油化工股份有限公司 | Silicon-containing wastewater treatment method, silicon-containing wastewater utilization system, molecular sieve preparation method and molecular sieve preparation system |
| CN106542543A (en) * | 2016-10-17 | 2017-03-29 | 中国石油化工股份有限公司 | The clean preparation method of modenite |
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Application publication date: 20200505 |