CN112717879A - Modified X-type molecular sieve hydrogen peroxide working solution regenerant, preparation method and application thereof - Google Patents
Modified X-type molecular sieve hydrogen peroxide working solution regenerant, preparation method and application thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
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- 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
- C01B39/20—Faujasite type, e.g. type X or Y
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Abstract
The invention discloses a modified X-type molecular sieve hydrogen peroxide working solution regenerant, a preparation method and application thereof. The regenerant of the invention is a spherical or strip regenerant prepared by modifying an X-type molecular sieve by using a binder and an auxiliary agent, wherein the auxiliary agent is water or dilute nitric acid. The regenerant provided by the invention obviously improves the regeneration effect of the working solution, and has the advantages of high static water balance adsorption capacity, difficult pulverization of the formed X-type molecular sieve, stable performance, long service life and low cost.
Description
Technical Field
The invention relates to the technical field of catalysts, in particular to a modified X-type molecular sieve hydrogen peroxide working solution regenerant, a preparation method and application thereof.
Background
The hydrogen peroxide is a strong oxidant, is an inorganic chemical raw material with high industrial application value, is widely applied to the fields of industry, medicine, military use and the like, and is green. Therefore, the demand of hydrogen peroxide is increasing day by day, and the synthesis process of hydrogen peroxide is widely researched in order to meet the huge market demand. The existing hydrogen peroxide preparation methods include anthraquinone method and direct hydrogen-oxygen synthesis method. The principle of anthraquinone method for industrially producing hydrogen peroxide is that alkyl anthraquinone is dissolved into working solution, hydrogenation reaction is carried out under the catalytic action of a catalyst taking nickel or palladium as an active component to generate alkyl anthraquinone, then the working solution containing the alkyl anthraquinone is oxidized to generate hydrogen peroxide and the alkyl anthraquinone, and then the working solution is extracted to obtain hydrogen peroxide solution and the working solution. The principle of the direct hydrogen-oxygen combination method is that a reaction medium and a catalyst are added into a high-pressure reactor, a mixed gas of hydrogen, oxygen and nitrogen in a certain proportion is introduced under the condition of continuous stirring, and the hydrogen peroxide can be generated through reaction at a certain temperature and under a certain pressure. The direct hydrogen-oxygen synthesis method has the defects of low product content and harsh conditions, and uses the mixed gas of hydrogen and oxygen, so the mixed gas has high risk, and the anthraquinone method is often selected industrially to prepare the hydrogen peroxide.
The principle of anthraquinone method for industrially producing hydrogen peroxide is that alkyl anthraquinone is dissolved into working solution, hydrogenation reaction is carried out under the catalytic action of a catalyst taking nickel or palladium as an active component to generate alkyl anthraquinone, then the working solution containing the alkyl anthraquinone is oxidized to generate hydrogen peroxide and the alkyl anthraquinone, and then the working solution is extracted to obtain hydrogen peroxide solution and the working solution. The anthraquinone process for producing hydrogen peroxide carrier, i.e. alkyl anthraquinone and tetrahydro alkyl anthraquinone, but because alkyl anthraquinone is continuously and cyclically subjected to hydrogenation reaction and oxidation reaction in the process of preparing hydrogen peroxide by anthraquinone process, various accompanying side reactions can not be avoided, some anthraquinone derivatives are generated, and substances which can not react to generate hydrogen peroxide are generated, and these substances are collectively called degradation products. The degradation of the alkylanthraquinone is divided into hydrogenation degradation and oxidation degradation, wherein the hydrogenation degradation comprises deep hydrogenation and carbonyl hydrogenolysis of anthraquinone aromatic rings, and the oxidation degradation is that the hydrogenated anthraquinone is subjected to oxidation reaction to generate anthraquinone epoxy compounds or acid anhydride substances. When the degradation product is accumulated to a certain concentration, the content of effective alkylanthraquinone in the working solution is reduced, the reaction efficiency is reduced, the loss is increased, and meanwhile, the degradation of the alkylanthraquinone can influence the property of the working solution, so that the density of the working solution is increased, the viscosity is increased, the operation load is increased, the energy consumption is increased, and the reaction can be stopped seriously. Therefore, the degradation and regeneration of organic matters such as anthraquinone and the like in the process of preparing hydrogen peroxide by the anthraquinone method are important factors influencing the production. The invention provides a regenerant for regenerating hydrogen peroxide working solution by using a modified X-type molecular sieve, which has the advantages of ideal regeneration effect, stable performance, simple preparation, low cost and easy preparation.
Patent CN 101554996A proposes a preparation method of hydrogen peroxide working solution regenerant, which adopts calcium oxide as an active component, and the component proportion is as follows: 1 to 99 percent of calcium oxide, the balance of alkaline oxide, preferably 50 to 70 percent of calcium oxide, and the balance of alkaline oxide. The method has the advantages of high calcium oxide content, no bonding with alkaline oxides, direct mixing, low strength, instability, easy dispersion in working solution, blockage of production devices and production stop.
Patent 105174229B proposes a composite active regenerant for hydrogen peroxide working solution prepared by anthraquinone process and a preparation method thereof, the active regenerant comprises a two-layer or three-layer structure, wherein the two-layer structure comprises 50% -95% of active alumina on the outer surface layer, the balance of calcium oxide, 50% of calcium oxide on the core layer, 50% of silicon dioxide, and the three-layer structure comprises 50% -99% of active alumina on the outermost layer, 0-2.5% of alkali metal oxide, the balance of calcium oxide, 50% -99% of calcium oxide on the centripetal layer, 0-2.5% of alkali metal oxide, the balance of silicon dioxide, 50% -99% of silicon oxide on the core layer, and the balance of calcium oxide. The hydrogen peroxide working solution regenerant prepared by the method comprises a multilayer structure, a core structure does not contain a binder, the structure is unstable, in addition, the multilayer structure ensures that the regeneration effect is not thorough, the regeneration amount of the working solution is limited, and the alkalinity of the working solution is increased due to the long-term use of the regenerant.
Patent CN 105152137B proposes a hydrogen peroxide working solution regenerant in a hydrogen peroxide preparation process by an anthraquinone method and a preparation method thereof, wherein the regenerant comprises: 10-80% of alumina powder, 10-80% of magnesium oxide powder, 1-112% of sesbania powder, gamma-type aluminum oxide and cubic magnesium oxide powder. The aluminum oxide is used as a regenerant, the regeneration effect is not ideal, a large amount of anthraquinone degradation products still exist after treatment, the service life of the regenerant is short, the regenerant needs to be replaced, and the waste of the regenerant is caused.
Disclosure of Invention
Based on the problems, the invention aims to provide a modified X-type molecular sieve hydrogen peroxide working solution regenerant and regenerate hydrogen peroxide working solution by using the same. The regenerant provided by the invention obviously improves the regeneration effect of the working solution, and has the advantages of high static water balance adsorption capacity, difficult pulverization of the formed X-type molecular sieve, stable performance, long service life and low cost.
The raw materials of the regenerant comprise an X-type molecular sieve, a binder and an auxiliary agent, wherein the auxiliary agent is water or dilute nitric acid, the X-type molecular sieve is a formed molecular sieve, the concentration of the dilute nitric acid is 1-15%, and the regenerant is spherical or strip-shaped.
Preferably, the molecular sieve is a NaX type molecular sieve.
Further preferably, the binder is one or more of silica sol, alumina powder, aluminum sol and pseudo-boehmite.
More preferably, the mass percentages of the raw materials in the regenerant are as follows:
50-90% of NaX type molecular sieve, 10-30% of binder and the balance of auxiliary agent.
The invention also aims to provide a preparation method of the modified X-type molecular sieve hydrogen peroxide working solution regenerant, which comprises the following steps:
step 1, weighing a molecular sieve, a binder and an auxiliary agent according to a proportion;
step 2, fully mixing the molecular sieve and the binder, and then adding an auxiliary agent to carry out a rolling ball or extruding process to obtain a spherical or strip material;
3, sieving the prepared spherical or strip-shaped material to remove powder and part of undesirable materials, and drying the sieved and formed material for 4-24 hours at the temperature of 30-130 ℃;
and 4, roasting the dried spherical or strip-shaped material for 4-10h at the temperature of 500-600 ℃ to finally obtain the spherical or strip-shaped hydrogen peroxide working solution regenerant.
Preferably, when the mixed material is subjected to the rolling ball process in the step 2, the adopted auxiliary agent is water, and when the mixed material is subjected to the strip extrusion process in the step 2, the adopted auxiliary agent is dilute nitric acid.
The invention also provides an application of the modified X-type molecular sieve hydrogen peroxide working solution regenerant, and specifically comprises the steps of adding 1-20 wt% of the regenerant into hydrogenated and degraded hydrogen peroxide working solution, and reacting for 2-6h in a water bath constant temperature oscillator at the temperature of 40-80 ℃.
Preferably, the hydrogen degradation hydrogen peroxide working solution is prepared by dissolving 140g/L of 2-Ethyl Anthraquinone (EAQ) in 2L of 75 volume ratio: 25 of heavy Aromatic Hydrocarbon (AH) and trioctyl phosphate (TOP); adding the dissolved materials and 1g of palladium catalyst into an autoclave, sealing the autoclave, replacing the autoclave for 3 times by hydrogen, introducing the hydrogen to heat the autoclave in a water bath under the pressure of 1MPa, heating the autoclave to 60 ℃, preserving the heat for 30min, and finally cooling and filtering to obtain the hydrogen degradation hydrogen peroxide working solution.
Preferably, the oscillation frequency of the oscillator is 100-250 rpm.
Compared with the prior art, the invention has the following beneficial effects:
the invention uses X-type molecular sieve as raw material, and the modified X-type molecular sieve with strong adsorption property and high stability is prepared by modifying the X-type molecular sieve with binder. The method is used for regenerating the hydrogen peroxide working solution, so that the regeneration effect of the working solution is improved, the static water balance adsorption capacity is high, the formed X-type molecular sieve is not easy to pulverize, the performance is stable, the service life is long, and the cost is low.
Detailed Description
The present invention will be further described with reference to the following specific examples. The hydrogenization degradation hydrogen peroxide working solution adopted in the following examples is prepared by dissolving 140g/L of 2-Ethyl Anthraquinone (EAQ) in 2L of 75 volume ratio: 25 of heavy Aromatic Hydrocarbon (AH) and trioctyl phosphate (TOP); adding the dissolved materials and 1g of palladium catalyst into an autoclave, sealing the autoclave, replacing the autoclave for 3 times by hydrogen, introducing the hydrogen to heat the autoclave in a water bath under the pressure of 1MPa, heating the autoclave to 60 ℃, preserving the heat for 30min, finally cooling and filtering to obtain the catalyst. Meanwhile, the X-type molecular sieve adopted in the following examples is NaX molecular sieve.
Example 1
1) Modified X-type molecular sieve regenerant:
step 1, weighing the following raw materials in percentage by mass: 80 percent of X-type molecular sieve, 10 percent of sesbania powder and 5 percent of silica sol with the concentration of 30 percent as a binder, and 5 percent of water as an auxiliary agent
Step 2, fully mixing the molecular sieve and the binder for 1h, transferring the mixture into a disc granulator, and spraying auxiliary agent water to roll balls to obtain material particles;
and 3, sieving the prepared material particles, removing small particles and powder, drying at the temperature of 120 ℃ for 6 hours, and roasting at the temperature of 550 ℃ for 4 hours to obtain the spherical hydrogen peroxide working solution regenerant.
2) Application of regenerant in regeneration of hydrogen peroxide working solution prepared by anthraquinone process
Measuring 200ml of hydrogen degradation hydrogen peroxide working solution, adding the hydrogen degradation hydrogen peroxide working solution into a triangular flask, then adding 10g of spherical modified X-type molecular sieve regenerant, sealing the triangular flask, placing the sealed triangular flask into a water bath constant-temperature oscillator, adjusting the water bath temperature to 50 ℃, the oscillation frequency to 150rpm, regenerating for 4 hours, taking out the triangular flask after regeneration is finished, cooling to room temperature, and taking the regenerated working solution for quantitative analysis.
Example 2
1) Modified X-type molecular sieve regenerant:
step 1, weighing the following raw materials in percentage by mass: 75 percent of X-type molecular sieve, 10 percent of sesbania powder and 8 percent of silica sol with the content of 30 percent as a binder, and 7 percent of water as an auxiliary agent
Step 2, fully mixing the molecular sieve, sesbania powder and silica sol for 1h, then transferring the mixture into a disc granulator, and spraying auxiliary agent water to roll balls to obtain material particles;
and 3, sieving the prepared material particles, removing small particles and powder, drying at the temperature of 120 ℃ for 6 hours, and roasting at the temperature of 550 ℃ for 4 hours to obtain the spherical hydrogen peroxide working solution regenerant.
2) Application of regenerant in regeneration of hydrogen peroxide working solution prepared by anthraquinone process
Measuring 200ml of hydrogen-degraded hydrogen peroxide working solution, adding the hydrogen-degraded hydrogen peroxide working solution into a triangular flask, then adding 20g of regenerant, sealing the triangular flask, placing the sealed triangular flask into a water bath constant-temperature oscillator, adjusting the water bath temperature to 50 ℃, adjusting the oscillation frequency to 150rpm, regenerating for 4 hours, taking out the triangular flask after regeneration is finished, cooling to room temperature, and taking the regenerated working solution for quantitative analysis.
Example 3
1) Modified X-type molecular sieve regenerant
Step 1, weighing the following raw materials in percentage by mass: mixing a 50% X-type molecular sieve, 25% alumina, 34% dilute nitric acid solution with the concentration of 7.6% and 1% sesbania powder, and transferring the mixture to a kneader for mixing;
step 2, homogenizing the dilute nitric acid solution, adding the dilute nitric acid solution into the materials, and continuously kneading the materials through a kneading machine to mix the materials;
step 3, extruding the uniformly mixed materials through a strip extruding machine;
and 4, airing the strip-shaped material for 12 hours at room temperature, and finally roasting for 4 hours at the temperature of 550 ℃ to obtain the strip-shaped hydrogen peroxide working solution regenerant.
2) Application of regenerant in regeneration of hydrogen peroxide working solution prepared by anthraquinone process
Measuring 200ml of hydrogen-degraded hydrogen peroxide working solution, adding the hydrogen-degraded hydrogen peroxide working solution into a triangular flask, then adding 20g of regenerant, sealing the triangular flask, placing the sealed triangular flask into a water bath constant-temperature oscillator, adjusting the water bath temperature to 50 ℃, adjusting the oscillation frequency to 150rpm, regenerating for 4 hours, taking out the triangular flask after regeneration is finished, cooling to room temperature, and taking the regenerated working solution for quantitative analysis.
Example 4
1) Modified X-type molecular sieve regenerant:
step 1, weighing the following raw materials in percentage by mass: mixing a 55% X-type molecular sieve, 15% alumina, 28% dilute nitric acid solution with the concentration of 6.96% and 2% sesbania powder, and transferring the mixture to a kneader for mixing;
step 2, adding a dilute nitric acid solution into the materials, and continuously kneading the materials through a kneading machine to mix the materials;
step 3, extruding the uniformly mixed materials through a strip extruding machine;
and step (3) airing the strip-shaped material for 12 hours at room temperature, and finally roasting the strip-shaped material for 4 hours at the temperature of 550 ℃ to obtain the strip-shaped hydrogen peroxide working solution regenerant.
2) Application of regenerant in regeneration of hydrogen peroxide working solution prepared by anthraquinone process
Measuring 200ml of hydrogen degradation hydrogen peroxide working solution, adding the hydrogen degradation hydrogen peroxide working solution into a triangular flask, then adding 20g of regenerant, sealing the triangular flask, placing the sealed triangular flask into a water bath constant temperature oscillator, adjusting the water bath temperature to 50 ℃, the oscillation frequency to 150rpm, regenerating for 4 hours, taking out the triangular flask after regeneration is finished, cooling to room temperature, and taking the regenerated working solution for quantitative analysis
Comparative example 1
Measuring 200ml of hydrogen-degraded hydrogen peroxide working solution, adding the hydrogen-degraded hydrogen peroxide working solution into a triangular flask, directly sealing the triangular flask without adding a regenerant, placing the sealed triangular flask into a water bath constant-temperature oscillator, adjusting the water bath temperature to 50 ℃, the oscillation frequency to 150rpm, regenerating for 4 hours, taking out the triangular flask after regeneration is finished, cooling to room temperature, and taking the regenerated working solution for quantitative analysis.
The working fluids obtained after the regeneration of examples 1 to 4 and comparative example 1 were examined, and the examination results are shown in table 1.
TABLE 1
The experimental results show that the modified X-type molecular sieve regenerant can achieve the aim of carrying out regeneration reaction on the working solution for preparing hydrogen peroxide by an anthraquinone method.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (9)
1. The regeneration agent for the modified X-type molecular sieve hydrogen peroxide working solution is characterized in that raw materials of the regeneration agent comprise a molecular sieve, a binder and an auxiliary agent, the auxiliary agent is water or dilute nitric acid, the concentration of the dilute nitric acid is 1-15%, and the regeneration agent is spherical or strip-shaped.
2. The modified X-type molecular sieve hydrogen peroxide working solution regenerant as claimed in claim 1, wherein the molecular sieve is NaX molecular sieve.
3. The regeneration agent of the modified X-type molecular sieve hydrogen peroxide working solution as claimed in claim 2, wherein the binder is one or more of silica sol, alumina powder, alumina sol, pseudo-boehmite, sesbania powder.
4. The regeneration agent of the modified X-type molecular sieve hydrogen peroxide working solution according to claim 3, wherein the regeneration agent comprises the following raw materials in percentage by mass:
50-90% of NaX type molecular sieve, 10-30% of binder and the balance of auxiliary agent.
5. The preparation method of the modified X-type molecular sieve hydrogen peroxide working solution regenerant according to any one of claims 1-4, characterized by comprising the following steps:
step 1, weighing a NaX type molecular sieve, a binder and an auxiliary agent in proportion;
step 2, mixing the NaX type molecular sieve and the binder, and then adding the auxiliary agent to roll the ball or extrude the ball into strips;
step 3, sieving the prepared material particles to remove powder and small particles, and then drying the sieved molding material for 4-24 h at the drying temperature of 30-130 ℃;
and 4, roasting the dried and molded material at the roasting temperature of 500-600 ℃ for 4-10h to obtain the spherical or strip-shaped modified hydrogen peroxide working solution regenerant.
6. The preparation method according to claim 5, wherein when the mixed raw materials are extruded into strips in the step 2, the adopted auxiliary agent is dilute nitric acid; when the mixed raw materials are rolled in the step 2, the adopted auxiliary agent is water.
7. The use of the regenerant for the modified X-type molecular sieve hydrogen peroxide working solution according to any one of claims 1 to 4, wherein 1 to 20 wt% of the regenerant is added to the hydrogen degraded hydrogen peroxide working solution, and the reaction is carried out in a water bath constant temperature oscillator at a temperature of 40 to 80 ℃ for 2 to 6 hours.
8. The use according to claim 1, wherein the hydrogen degraded hydrogen peroxide working solution is prepared by dissolving 140g/L of 2-Ethyl Anthraquinone (EAQ) in 2L of 75: 25 of heavy Aromatic Hydrocarbon (AH) and trioctyl phosphate (TOP); adding the dissolved materials and 1g of palladium catalyst into an autoclave, sealing the autoclave, replacing the autoclave for 3 times by hydrogen, introducing the hydrogen to heat the autoclave in a water bath under the pressure of 1MPa, heating the autoclave to 60 ℃, preserving the heat for 30min, and finally cooling and filtering to obtain the hydrogen degradation hydrogen peroxide working solution.
9. The use according to claim 7, wherein the oscillation frequency of the oscillator is 100-250 rpm.
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Application publication date: 20210430 |