Microcrystalline wax hydrofining catalyst, preparation method thereof and method for preparing microcrystalline wax by using microcrystalline wax hydrofining catalyst

The metal oxide is loaded with a modified silicon-aluminum powder support and impregnation method to prepare an efficient microcrystalline wax hydrorefining catalyst, which solves the problem of difficulty in removing impurities in microcrystalline waxes in the prior art, and realizes the production of high-purity and high-quality microcrystalline waxes.

CN119838615APending Publication Date: 2025-04-18FUSHUN XINRUI CATALYST
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Patent Information

Application Number
CN202510074739.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-01-17
Publication Date
2025-04-18

AI Technical Summary

Technical Problem

The prior art is difficult to effectively remove impurities in microcrystalline waxes, resulting in their quality not meeting the standards and cannot meet higher quality standards.

Method used

Modified silicon-aluminum powder was used as the catalyst support, and metal oxides such as tungsten, cobalt, nickel and phosphorus were loaded through the impregnation method to prepare a microcrystalline wax hydrofining catalyst with high specific surface area and pore volume.

Benefits of technology

It improves the activity and selectivity of the catalyst, enhances the ability to remove impurities, and produces high-purity, high-quality microcrystalline waxes, meeting stricter quality standards.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention provides a microcrystalline wax hydrofining catalyst, a preparation method thereof and a method for preparing microcrystalline wax by using the microcrystalline wax hydrofining catalyst, and relates to the field of catalysts. The preparation method comprises the following steps: dropwise adding aluminum sulfate into water at 60-70 DEG C, controlling the pH value of a system to be 6-7, then dropwise adding water glass and ammonia water, and controlling the pH value of the system to be 8-8.5; circularly dropwise adding aluminum sulfate, water glass and ammonia water, reacting at 75-78 DEG C, then carrying out constant-temperature aging treatment, carrying out solid-liquid separation, and washing the solid to obtain modified silicon-aluminum powder; mixing the modified silicon-aluminum powder, organic acid, inorganic acid, an extrusion aid and water, molding, drying and roasting to obtain a catalyst carrier; tungsten salt, cobalt salt, nickel salt, phosphoric acid and water are mixed to prepare steeping liquor, the catalyst carrier is added into the steeping liquor to be steeped, and drying and roasting are conducted to obtain the microcrystalline wax hydrofining catalyst. The catalyst provided by the invention is suitable for inferior microcrystalline wax raw materials with high impurity content, and the obtained microcrystalline wax is good in quality.
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Description

Technical Field

[0001] The present application relates to the field of catalysts, and in particular to a microcrystalline wax hydrogenation refining catalyst, a preparation method thereof, and a method for preparing microcrystalline wax using the same. Background Art

[0002] Microcrystalline wax is a product obtained by solvent deasphalting, solvent refining, dewaxing, and deoiling of vacuum residue of paraffin-based crude oil. Its main components are branched saturated hydrocarbons of C31-70. Unrefined microcrystalline wax contains more sulfur, nitrogen, oxygen heteroatom compounds and aromatic compounds, as well as a small amount of high molecular weight polycyclic compounds such as colloids and asphaltene. Hydrogenation refining is currently the main method for producing high-quality microcrystalline wax. Refined microcrystalline wax products have the characteristics of low hardness, good flexibility, and large elongation. With the development of science and technology, microcrystalline wax is widely used in various special wax blending, grease thickeners, daily chemical raw materials, medicine and food packaging.

[0003] The characteristics of microcrystalline wax determine its high melting point, good gloss, tight structure, light color, etc., which makes it not only able to increase the melting point of other low-grade waxes, but also improve the special properties of coarse waxes. In addition, microcrystalline wax has high transparency, chemical stability, and emulsification. It can form a stable paste with a variety of solvents and wax products, and is suitable for a variety of chemical fields. With the rapid iteration of products required by the market, there are extremely strict regulations and requirements for the quality of microcrystalline wax for daily chemical raw materials, food packaging, and medicine. In order to meet the needs of chemical, pharmaceutical and other industries for high-quality microcrystalline wax, microcrystalline wax needs to be deeply hydrogenated and refined. The key to hydrogenation refining is to develop high-performance hydrogenation catalysts. Through the catalyst hydrogenation refining process, the purity and quality of microcrystalline wax can be improved, the impurity content can be reduced, and high-quality microcrystalline wax can be produced to meet higher quality standards. Summary of the invention

[0004] The purpose of the present application is to provide a microcrystalline wax hydrorefining catalyst and a preparation method thereof and a method for preparing microcrystalline wax using the same, so as to solve the above problems.

[0005] To achieve the above objectives, this application adopts the following technical solutions:

[0006] A method for preparing a microcrystalline wax hydrorefining catalyst comprises:

[0007] Preparation of modified silicon-aluminum powder: adding aluminum sulfate dropwise to 60-70°C water, during which the pH value of the system is controlled to be 6-7, then adding water glass and ammonia water dropwise, during which the pH value of the system is controlled to be 8-8.5; cyclically adding aluminum sulfate, water glass and ammonia water dropwise, maintaining the reaction at 75-78°C, then performing constant temperature aging treatment, solid-liquid separation, and washing the solid to obtain the modified silicon-aluminum powder;

[0008] Preparation of the catalyst carrier: the modified silicon-aluminum powder, organic acid, inorganic acid, extrusion aid and water are mixed, and then molded, dried and calcined to obtain the catalyst carrier;

[0009] Preparation of microcrystalline wax hydrorefining catalyst: tungsten salt, cobalt salt, nickel salt, phosphoric acid and water are mixed to prepare an impregnation solution, and then the catalyst carrier is added to the impregnation solution for impregnation. After the impregnation is completed, a second drying and a second calcination are performed to obtain the microcrystalline wax hydrorefining catalyst.

[0010] Preferably, the ratio of the aluminum sulfate, the water glass and the ammonia water is 3-5:1-2:5-8.

[0011] Preferably, the organic acid comprises glacial acetic acid and / or citric acid, the inorganic acid comprises nitric acid and / or phosphoric acid, and the extrusion aid comprises sesbania powder and / or silica sol.

[0012] Preferably, the mass ratio of the modified silica-alumina powder, the organic acid, the inorganic acid and the extrusion aid is in the range of 70-90: 2-8: 3-10: 2-10.

[0013] Preferably, the temperature of the first drying is 100-120°C, and the time is 3-4h; the heating rate of the first calcination is 100-120°C / h, the maximum temperature is 780-820°C, and the insulation time is 2-2.5h.

[0014] Preferably, calculated as metal oxides, each 100 ml of the impregnation solution contains: 18-22 g of tungsten oxide, 3-5 g of nickel oxide, and 2-3.5 g of cobalt oxide;

[0015] Each 100 ml of the impregnation solution contains 2-2.5 g of phosphorus.

[0016] Preferably, the temperature of the second drying is 100-120°C, and the time is 3-4h; the heating rate of the second calcination is 100-120°C / h, the maximum temperature is 530-570°C, and the insulation time is 2-2.5h.

[0017] The present application also provides a microcrystalline wax hydrorefining catalyst, which is prepared using the preparation method of the microcrystalline wax hydrorefining catalyst.

[0018] Preferably, the bulk density of the microcrystalline wax hydrorefining catalyst is 0.75-0.80 g / ml 3 The crushing strength is not less than 120N / cm, and the specific surface area is not less than 160m 2 / g, pore volume not less than 0.45ml / g;

[0019] The tungsten content is 18-22wt%, the nickel content is 3-5wt%, the cobalt content is 2-3.5wt%, and the phosphorus content is 2-2.5wt%.

[0020] The present application also provides a method for preparing microcrystalline wax using the microcrystalline wax hydrogenation refining catalyst, comprising:

[0021] The microcrystalline wax raw material is added to a first-stage hydrogenation reactor for a first-stage hydrogenation reaction, and then sent to a second-stage hydrogenation refining reactor for a second-stage hydrogenation reaction to obtain a microcrystalline wax product;

[0022] The first stage hydrogenation reactor and the second stage hydrogenation refining reactor are filled with the microcrystalline wax hydrogenation refining catalyst;

[0023] The reaction temperature of the first stage hydrogenation reaction is 300-320°C, the temperature of the second stage hydrogenation reaction is 260-280°C, the reaction pressure is 13-15MPa, and the volume space velocity is 0.15-0.3m 3 / h, hydrogen to wax ratio is 800-1000.

[0024] Compared with the prior art, the beneficial effects of this application include:

[0025] The preparation method of the microcrystalline wax hydrorefining catalyst provided in the present application is to prepare a catalyst carrier by preparing modified silicon aluminum powder, improve the pore volume and specific surface area of ​​the catalyst, and improve the uniformity and dispersibility of the content of the active component of the catalyst; the loading of active metals enables the catalyst to obtain a suitable reaction temperature to meet the needs of microcrystalline wax hydrorefining; at the same time, the catalyst has weak surface acidity to prevent the oil content from rising due to the cracking of raw material molecules, and in view of the characteristics that the hydrogenation reaction of macromolecular impurities such as condensed aromatic hydrocarbons in the microcrystalline wax raw material is controlled by internal diffusion, the screened active components are composed of W, Co, and Ni metal oxides; the use of the impregnation method makes the active metal loading more uniform. Adding P as an auxiliary agent allows synergistic effects between the active metal and the auxiliary agent, and between the active metal and the active metal, resulting in a low polymerization rate of the catalyst, and the catalyst has good selectivity and stability.

[0026] The microcrystalline wax hydrogenation refining catalyst provided in the present application has a microcrystalline wax hydrogenation catalyst with a higher specific surface area and pore volume. The catalyst has a higher ability to remove impurities and also has a higher mechanical strength. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for use in the embodiments will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present application and therefore should not be regarded as limiting the scope of the present application.

[0028] Figure 1 This is a photo of the microcrystalline wax hydrorefining catalyst prepared in Example 1. DETAILED DESCRIPTION

[0029] First, the technical solution of this application is described as a whole, as follows:

[0030] One of the purposes of the present application is to provide a carrier made of special modified silica-alumina powder for use in microcrystalline wax catalyst.

[0031] Catalyst carrier preparation:

[0032] First, prepare special modified silicon aluminum powder: aluminum sulfate, 30% water glass, 22% to 25% ammonia water in different proportions, divide 5 to 6 portions into the synthesis kettle in turn, add a certain proportion of water into the synthesis kettle, heat it to 65℃±5℃, add aluminum sulfate, adjust pH=6~7, and then add 30% water glass and 22% to 25% ammonia water at the same time, control the drop speed of the two solutions, and strictly control pH=8~8.5, and use pH control to adjust the amount of solution added. Each portion of aluminum sulfate, 30% water glass, and 22% to 25% ammonia water are added in turn, and the reaction temperature is controlled at 75 to 78℃. After the addition is complete, the temperature is kept constant for 50 minutes, the mother liquor is filtered, washed with water twice, and then washed with 1% ammonia water for many times. No sulfate ions can be detected, and the washing is completed, and the mixture is dried, roasted, and ground for standby use.

[0033] The second step is the preparation of the carrier: add an appropriate amount of organic acid (such as glacial acetic acid, citric acid, etc.), inorganic acid, extrusion aid (such as sesbania powder, etc.) and water to the qualified silicon aluminum powder, knead it, extrude it into strips, dry it, and bake it to make the catalyst carrier. The carrier pore volume ≥ 0.8ml / g, specific surface area ≥ 320m 2 / g, the modified special silicon aluminum powder effectively improves the uniformity and dispersibility of the content of the active components of the catalyst.

[0034] The second object of the present application is to provide a catalyst for the properties of microcrystalline wax.

[0035] Microcrystalline wax hydrorefining requires a higher reaction temperature, so the catalyst should have weak surface acidity to prevent the oil content from rising due to the cracking of raw material molecules, and in view of the characteristics that the hydrogenation reaction of macromolecular impurities such as condensed aromatic hydrocarbons in the microcrystalline wax raw material is controlled by internal diffusion, the screened active components are composed of W, Co, and Ni metal oxides. The present application adopts an impregnation method to make the carrier of the purpose one carry active components and auxiliary components. According to the water absorption rate of the carrier and the designed active metal content, a certain concentration of impregnation liquid is prepared to make the impregnation liquid weakly acidic, and an equal volume impregnation method is adopted to mix the impregnation liquid and the carrier evenly. The catalyst preferably has W, Co, and Ni active components, and the addition of P auxiliary agent allows synergistic effects between the active metal and the auxiliary agent, and between the auxiliary agent and the auxiliary agent, so that the polymerization rate of the catalyst can be reduced to a low level, and the catalyst has good selectivity and stability.

[0036] The impregnated carrier loaded with different contents of active components and auxiliary components can be dried (dried) and calcined according to the usual operation. The preferred drying and calcining conditions of the present invention are to dry the impregnated catalyst at 100°C to 120°C for 3 to 4 hours, and then calcine at 530°C to 550°C for 2 to 2.5 hours to obtain the hydrogenation catalyst of the present invention.

[0037] Using the method of the present application, a pore volume greater than 0.45 mL / g and a specific surface area greater than 160 m 2 / g or even a microcrystalline wax hydrogenation catalyst with a higher specific surface area and pore volume. The catalyst has a higher ability to remove impurities and also has a higher mechanical strength (the lateral pressure strength can reach 120-180N / cm or higher). Its physical and chemical indicators are shown in Table 1.

[0038] Table 1 Physical and chemical indicators of catalyst

[0039] Analyze Project Quality indicators Appearance Shamrock Specification / mm Φ(1.4~1.6)*(3~12) <![CDATA[Bulk density / g.ml -1 > 0.75±0.05 <![CDATA[Crushing strength / N.cm -1 > ≥120 <![CDATA[Specific surface area / m 2 .g -1 > ≥160 <![CDATA[Pore volume / ml.g -1 > ≥0.45 Catalyst composition / wt% W 18~22 Ni 3~5 Co 2~3.5 Additives 2~2.5

[0040] The third purpose of this application is to provide a process flow for microcrystalline wax.

[0041] The method of this application uses crude microcrystalline wax as raw material and adopts two-stage hydrogenation technology. The product meets the requirements of food wax and the quality index reaches the level of high-quality microcrystalline wax in the current international market. Microcrystalline wax hydrogenation refining adopts a two-stage series hydrogenation process, one stage is filled with the main catalyst, and the second stage is filled with part of the main agent and dechlorination agent (volume ratio 3:1). The optimized process conditions are shown in Table 2.

[0042] Table 2 Microcrystalline wax process conditions

[0043] Process conditions One section Second paragraph <![CDATA[Space velocity per hour -1 > 0.15-0.3 0.15-0.3 Reaction temperature / ℃ 300~320 260~280 Reaction pressure / MPa 13-15 13-15 Hydrogen wax volume ratio 800-1000:1 800-1000:1

[0044] In view of the characteristics of large relative molecular mass, high content of polycyclic aromatic hydrocarbons and great difficulty in hydrogenation refining of microcrystalline wax raw materials, the catalyst adopts a special modified silicon aluminum powder carrier preparation process. A variety of active component loading technologies make the active metals evenly dispersed. The catalyst has a large specific surface, large pore size and pore volume, which is suitable for the characteristics of long-chain and macromolecular structure of microcrystalline wax. The improvement of catalyst performance can improve the hydrogenation selectivity of the catalyst. Shorten the preparation process and improve environmental protection and economy. Compared with the existing microcrystalline wax hydrogenation catalyst, its preparation process is short, easy to operate, low production cost, and the new catalytic carrier material is used to impregnate the W-Ni-P-Co multi-component solution in one step, which greatly improves the performance of the catalyst. The catalyst is suitable for inferior microcrystalline wax raw materials of different grades and can be widely used in the hydrogenation refining of microcrystalline wax of different grades.

[0045] The two-stage hydrogenation process is used to improve the purity and quality of microcrystalline wax, reduce the impurity content, and produce high-quality microcrystalline wax under appropriate process conditions to meet higher quality index requirements for microcrystalline wax for food use. The environmentally friendly process can greatly reduce the impact on the environment, while further improving production efficiency and reducing production costs.

[0046] The embodiments of the present application will be described in detail below in conjunction with specific examples, but it will be appreciated by those skilled in the art that the following examples are only used to illustrate the present application and should not be considered as limiting the scope of the present application. If specific conditions are not specified in the examples, they are carried out according to normal conditions or the conditions recommended by the manufacturer. If the manufacturer is not specified for the reagents or instruments used, they are all conventional products that can be purchased commercially.

[0047] Example 1

[0048] ⑴. Synthesis of special modified silicon aluminum powder:

[0049] a. Aluminum sulfate 1012g + water to 5L;

[0050] b. 30% water glass 285ml + water to make up to 850ml;

[0051] c. 25% ammonia water 720ml + water to make up to 1.8L;

[0052] ①. Add 1L of water into the synthesis kettle and heat to 65℃±5℃.

[0053] ②. Divide a into 5 equal portions, 1000ml each; divide b into 5 equal portions, 170ml each; divide c into 5 equal portions, 360ml each.

[0054] ③. First slowly add 1 portion of solution a to adjust the pH to 6-7, then add solutions b and c at the same time, control the adding speed of the two solutions, and strictly control the pH to 8-8.5. Add one portion every 5 minutes, and always control the pH. Repeat this cycle until solutions a, b, and c are completely added. During this period, control the reaction temperature at 75-78°C and age at a constant temperature for 50 minutes.

[0055] ④. After filtering the mother liquor, wash it twice with 4L of water, and then wash it several times with 1% ammonia water. If no sulfate ions can be detected, the washing is completed, and then dry, roast and crush.

[0056] (2) Preparation of carrier:

[0057] Weigh 1000 g of the special modified silicon aluminum powder described in step ⑴, add 20 ml of glacial acetic acid, 65 ml of 21% nitric acid and 10 ml of phosphoric acid, an appropriate amount of field sesbania powder, silica sol, and water, mix well, extrude into a clover shape (ф1.6 mm), dry completely at room temperature, dry at 110°C for 2 hours, and then transfer to a high-temperature furnace, heat to 800°C at a heating rate of 120°C / h, and keep the temperature constant for 2 hours.

[0058] (3) Preparation of catalyst

[0059] Weigh 100 g of the carrier prepared in step (2), add 110 ml of a clear and transparent impregnation solution containing W-Ni-Co-P (each 100 ml of the solution contains 21 g WO3, 4.5 g NiO, 2 g CoO, and 2 g P), and soak at room temperature for 1 hour. After the obtained sample is completely dried at room temperature, it is dried at 120°C for 2 hours, and then transferred to a high-temperature furnace, heated to 550°C at a rate of 120°C / h, and kept at this temperature for 2 hours.

[0060] The photo of the microcrystalline wax hydrorefining catalyst prepared in Example 1 is as follows Figure 1 shown.

[0061] Comparative Example 1

[0062] (1) The steps for synthesizing special modified silicon aluminum powder are the same as those in Example 1.

[0063] (2) The steps for preparing the carrier are the same as those in Example 1, except that the ratio of the specially modified silicon aluminum powder to the commercially available alumina powder with large pore volume and specific surface area is 1:1.

[0064] (3) The catalyst impregnation and drying steps are the same as those in Example 1.

[0065] Comparative Example 2

[0066] (1) In the preparation of the carrier, no special modified silicon aluminum powder was used. Instead, commercially available alumina powder with large pore volume and specific surface area was used. The steps were the same as those in Example 1 to prepare the carrier of Comparative Example 1.

[0067] (2) The catalyst preparation is the same as in Example 1.

[0068] Comparative Example 3

[0069] (1) The preparation of the carrier is the same as in Example 1.

[0070] (2) Catalyst preparation: 110 ml of impregnation solution containing Mo-Ni-P was added to 100 g of the carrier, and the subsequent steps were the same as those in Example 1.

[0071] The physicochemical properties of the carriers and catalysts prepared in the above examples are listed in Table 3. From the data in Table 3, it can be seen that the catalyst prepared by the invention has a larger pore size and specific surface area after impregnation with a high metal content than the catalyst prepared by the carrier of Comparative Example 1, and is more conducive to the hydrogenation removal of condensed aromatic hydrocarbons, macromolecular impurities, etc.

[0072] Table 3 Physicochemical properties of catalyst samples

[0073]

[0074] The properties of a low-quality microcrystalline wax raw material used for catalyst activity evaluation, reaction process conditions, and quality indicators of the generated wax are shown in Table 4. The results of the evaluation of the 200ml small microcrystalline wax hydrorefining evaluation device (see Table 4) show the selectivity and activity of the hydrorefining catalyst. The main purpose of the catalyst is to remove polycyclic aromatic hydrocarbons and heterocyclic compounds such as sulfur, nitrogen, and oxygen that affect color and stability in the raw material without changing the main property indicators (such as drop melting point, needle penetration, viscosity, etc.). Therefore, the catalyst active metal and higher metal dispersion can provide more uniform active centers, and the refining effect is significant.

[0075] Table 4 Microcrystalline wax hydrogenation evaluation results

[0076]

[0077] Table 5 shows the hydrogenation activity data of the catalyst of the present invention when used with different grades of microcrystalline wax raw materials. The raw materials are dark in color and have a high impurity content, and are typical inferior wax materials. From the data (see Table 5), it can be concluded that the catalyst has a wide range of applicability. The catalyst prepared by the method of the present invention is suitable for processing inferior microcrystalline wax raw materials of different grades and high impurity content, thereby increasing profit margins.

[0078] Table 5 Evaluation data of catalyst in different raw materials in Example 1

[0079]

[0080] Table 6 shows the product data of the catalyst of the present invention under different process conditions. The two-stage hydrogenation process is adopted. Appropriate process conditions are the guarantee of catalyst activity and stability. Under the premise of improving the purity and quality of microcrystalline wax, reducing the impurity content, producing high-quality microcrystalline wax, and meeting the higher quality index requirements of microcrystalline wax for food, reducing temperature and pressure, increasing air velocity, and using environmentally friendly process flow can greatly reduce the waste of resources, while further improving production efficiency and reducing production costs.

[0081] Table 6 Evaluation data of catalyst in Example 1 under different process conditions

[0082]

[0083]

[0084] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit it. Although the present application has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the aforementioned embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present application.

Claims

1. A method for preparing a microcrystalline wax hydrorefining catalyst, characterized in that: include: Preparation of modified silicon-aluminum powder: adding aluminum sulfate dropwise to 60-70°C water, during which the pH value of the system is controlled to be 6-7, then adding water glass and ammonia water dropwise, during which the pH value of the system is controlled to be 8-8.5; cyclically adding aluminum sulfate, water glass and ammonia water dropwise, maintaining the reaction at 75-78°C, then performing constant temperature aging treatment, solid-liquid separation, and washing the solid to obtain the modified silicon-aluminum powder; Preparation of the catalyst carrier: the modified silicon-aluminum powder, organic acid, inorganic acid, extrusion aid and water are mixed, and then molded, dried and calcined to obtain the catalyst carrier; Preparation of microcrystalline wax hydrorefining catalyst: tungsten salt, cobalt salt, nickel salt, phosphoric acid and water are mixed to prepare an impregnation solution, and then the catalyst carrier is added to the impregnation solution for impregnation. After the impregnation is completed, a second drying and a second calcination are performed to obtain the microcrystalline wax hydrorefining catalyst.

2. The method for preparing a microcrystalline wax hydrorefining catalyst according to claim 1, characterized in that: The molar ratio of the aluminum sulfate, the water glass and the ammonia water is 3-5:1-2:5-8.

3. The method for preparing a microcrystalline wax hydrorefining catalyst according to claim 1, characterized in that: The organic acid includes glacial acetic acid and / or citric acid, the inorganic acid includes nitric acid and / or phosphoric acid, and the extrusion aid includes sesbania powder and / or silica sol.

4. The method for preparing a microcrystalline wax hydrorefining catalyst according to claim 3, characterized in that: The mass ratio of the modified silicon aluminum powder, the organic acid, the inorganic acid and the extrusion aid is in the range of 70-90: 2-8: 3-10: 2-10.

5. The method for preparing a microcrystalline wax hydrorefining catalyst according to claim 1, characterized in that: The temperature of the first drying is 100-120° C., and the time is 3-4 hours; the heating rate of the first calcination is 100-120° C. / h, the maximum temperature is 780-820° C., and the insulation time is 2-2.5 hours.

6. The method for preparing a microcrystalline wax hydrorefining catalyst according to claim 1, characterized in that: Calculated as metal oxides, each 100 ml of the impregnation solution contains: 18-22 g of tungsten oxide, 3-5 g of nickel oxide, and 2-3.5 g of cobalt oxide; Each 100 ml of the impregnation solution contains 2 to 2.5 g of phosphorus.

7. The method for preparing a microcrystalline wax hydrorefining catalyst according to any one of claims 1 to 6, characterized in that: The temperature of the second drying is 100-120° C., and the time is 3-4 hours; the heating rate of the second roasting is 100-120° C. / h, the maximum temperature is 530-570° C., and the insulation time is 2-2.5 hours.

8. A microcrystalline wax hydrorefining catalyst, characterized in that: The catalyst is prepared by the method for preparing the microcrystalline wax hydrorefining catalyst according to any one of claims 1 to 7.

9. The microcrystalline wax hydrorefining catalyst according to claim 8, characterized in that: The bulk density of the microcrystalline wax hydrorefining catalyst is 0.75-0.80 g / ml 3 The crushing strength is not less than 120N / cm, and the specific surface area is not less than 160m 2 / g, pore volume not less than 0.45ml / g; The tungsten content is 18-22wt%, the nickel content is 3-5wt%, the cobalt content is 2-3.5wt%, and the phosphorus content is 2-2.5wt%.

10. A method for preparing microcrystalline wax using the microcrystalline wax hydrorefining catalyst according to claim 8 or 9, characterized in that: include: The microcrystalline wax raw material is added to a first-stage hydrogenation reactor for a first-stage hydrogenation reaction, and then sent to a second-stage hydrogenation refining reactor for a second-stage hydrogenation reaction to obtain a microcrystalline wax product; The first stage hydrogenation reactor and the second stage hydrogenation refining reactor are filled with the microcrystalline wax hydrogenation refining catalyst; The reaction temperature of the first stage hydrogenation reaction is 300-320°C, the temperature of the second stage hydrogenation reaction is 260-280°C, the reaction pressure is 13-15MPa, and the volume space velocity is 0.15-0.3m 3 / h, hydrogen to wax ratio is 800-1000.