CN102451691B - Preparation method of nickel-based hydrogenation catalyst - Google Patents
Preparation method of nickel-based hydrogenation catalyst Download PDFInfo
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Abstract
The invention discloses a preparation method of a nickel-based hydrogenation catalyst. The preparation method comprises the following steps that carrier alumina and /or silicon oxide, an active metal ingredient and an auxiliary agent ingredient are prepared into slurry; the slurry and a precipitator are added into a reactor in a parallel flow way and are prepared into a catalyst precursor; and the catalyst precursor, a peptizing agent and water are mixed, kneaded, molded, dried and calcined to form the nickel-based hydrogenation catalyst. Through the preparation method, the active metal ingredient can uniformly precipitate on the carrier so that high-uniformity uniformity of the active metal ingredient on the carrier is guaranteed. Through the parallel flow way for precipitation, a uniform precipitation environment in precipitation is obtained so precipitates having the same shape and size are obtained. The nickel-based hydrogenation catalyst obtained by the preparation method can be utilized for hydrogenation decoloration of C5 petroleum resin, C9 petroleum resin and C5-C9 mixed petroleum resin.
Description
Technical field
The present invention relates to a kind of preparation method of nickel-base hydrogenation catalyst, particularly for C
5petropols, C
9petropols and C
5, C
9blended hydrogenation of petroleum resin decolouring catalyst.
Background technology
Petropols are functional resins that a kind of relative molecular mass is lower, the characteristic having tackifying, caking property and mix with other resin.Be widely used in the fields such as coating, adhesive, printing-ink, rubber chemicals, paper additive.Petropols, according to the difference of raw materials for production and character, can be divided into C
5petropols, C
9petropols, C
5-C
9copolymerization oil tree etc.At present, the main source preparing Petropols is the accessory substance of petroleum cracking ethene, this byproduct is because of the difference of its cracking stock and cracking severity, output is generally 10% ~ 20% of ethylene product, due to cracking stock composition complexity and production technology and the production technology backwardness relatively of producing Petropols, cause that the color and luster of Petropols is dark, poor stability, especially the existence of double bond and phenyl ring have impact on the colourity of resin, stability and the compatibility with other resins, limits its range of application.Carrying out hydrogenation to Petropols is one of petroleum resin modified important means, namely Petropols are under the condition of hydrogen and catalyst, make double bond and part benzene ring hydrogenation in Petropols molecule saturated, be stripped of again the halogen element that Petropols remain in the course of the polymerization process, improve color and luster and the photo and thermal stability of Petropols, improve product quality, expand the range of application of Petropols.
Hydrogenation of petroleum resin catalyst adopts the noble metal such as palladium, platinum as catalyst activity component usually, and it can limit resin hydrocracking side reaction effectively.US 4,384,080 and US 4,952,639 describes the hydrogenation of petroleum resin method making hydrogenation catalyst with noble metals such as palladium, platinum, rhenium, rutheniums, and general employing single component metal is catalyst activity component.US 4,540,480 describes a kind of hydrogenation of petroleum resin method, and the active component of hydrogenation catalyst used therein adopts noble metal, and the carrier of catalyst is Al
2o
3, it is said that this catalyst has higher activity and longer service life; CN 02137114.8 discloses a kind of for by the hydrogenation catalyst of dicyclopentadiene petroleum resin Hydrogenation for dicyclopentadiene hydrogenated petroleum resin, this catalyst activity component is Pd and Pt, the content of Pd is 0.1wt% ~ 1.0wt%, the content of Pt is 0.05wt% ~ 0.50wt%, and catalyst carrier is γ-Al
2o
3, its specific area is 150 ~ 250m
2/ g, pore volume is 0.5 ~ 0.9mL/g, and this catalyst reaches ideal effect improving in the form and aspect of dicyclopentadiene petroleum resin.Although noble metal catalyst has stronger alkene, aromatic saturation ability, ideal effect is reached in hydrogenation of petroleum resin decolouring, but there is following shortcoming in noble metal catalyst: first, noble metal catalyst on preparation cost far away higher than non-precious metal catalyst; Secondly, noble metal catalyst is in use to the requirement of impurity content in raw material, particularly harsh especially to the content requirement of sulphur in raw material.Therefore, the hydrogenation process adopting noble metal catalyst to carry out must control the impurity content in raw material.
Nickel-base hydrogenation catalyst is cheap, activity is higher, has stronger alkene, aromatic saturation ability, simultaneously, effectively can make the organic compound hydrogenolysis containing the assorted element such as S, N, O in oil, there is the advantages such as process raw material range is wide, liquid yield is high, good product quality.At present, be that the nickel catalyst of carrier is also generally used with diatomite, wherein nickel content is generally 40% ~ 60%, and this catalyst can make adding hydrogen into resin degrade, and suitable hydrogenation degraded can make resin intersolubility improve.
The preparation method that nickel-base hydrogenation catalyst is general has: coprecipitation, mechanical mixing, infusion process etc.Coprecipitation is a kind of method two or more component simultaneously precipitated.Be characterized in once can obtaining several component, and the distribution of each component is more even simultaneously.When infusion process prepares high-nickel catalyst, for meeting catalyst content, in catalyst soakage process, need dipping, the drying of carrier being carried out to more than twice or twice, even roasting, makes catalyst strength sharply decline.The catalyst adopting the pore volume of mechanical mixing Kaolinite Preparation of Catalyst to be less than coprecipitation to prepare, this is owing to adding a large amount of active metal salts in catalyst preparation process, need to add a large amount of peptization acid during preparation to carry out peptization catalyst just can be made shaping smoothly, very large on the pore structure impact of catalyst; And adopt coprecipitation to prepare the catalyst of high tenor, effectively can overcome these problems, preparation flow is simple, is more conducive to the dispersion and the utilization rate that improve active metal.
CN200610064904.6 discloses applicable cracking C
9a kind of nickel series hydrogenating catalyst of cut fraction hydrogenation and preparation method thereof, CN200810113134.9 a kind of non-noble metal hydrogenation catalyst disclosing applicable hydrogenation of petroleum resin and preparation method thereof, these two kinds of catalyst all adopt coprecipitation method to prepare, under wherein the mixed solution of nickel salt and builder salts being heated to uniform temperature, add alkaline precipitating agent again, sediment makes catalyst through washing, dry, shaping and roasting.The preparation shortcoming of this catalyst is that precipitation process precipitation environment is instantaneously all not identical, and cause precipitated grain size to differ, the activity level affecting nickel plays, and reduces the activity of catalyst; Particularly CN200610064904.6 is in catalyst preparation process, and alumina catalyst support and active metal precipitate simultaneously, and active metal enters the lattice of aluminium oxide, causes active metal normally not play, reduces active utilization rate.
CN200610016260.3 discloses a kind of preparation method of the high-nickel catalyst for unsaturated vegetable and animals oils hydrogenation and removing double bond, it is characterized in that alkaline sedimentation agent solution is put into reactor is heated to 60 ~ 70 DEG C, stirring adds soluble nickel salting liquid and precipitates, add alumina support after nickel salt solution adds, stir after 0.5 ~ 1.0 hour wash, dry, pulverize and roasting high-nickel catalyst.The preparation shortcoming of this catalyst is: first, in precipitation process, acid nickel salt solution adds in the precipitant solution of alkalescence, cause the precipitation environment of the moment of the precipitation process in reactor all not identical, namely precipitation reaction pH value in a kettle. descendingly to be carried out in variation, thus cause precipitated grain size to differ, affect the performance of the activity level of nickel, reduce the activity of catalyst; Secondly, add alumina support after precipitation terminates, this process belongs to two kinds of solid matters and mixes, and is unfavorable for the dispersion of nickel sediment at carrier surface, reduces the utilization rate of active metal.
US 4042532 discloses a kind of preparation method of thermally-stabilised good Ni-Al catalyst, the method is that nickel is mixed with nickel ammonium salt aqueous solution, saturated dipping aluminium hydroxide again, then at high temperature decompose in the duct and space that ammonium compound makes nickel be deposited in aluminium hydroxide, make the skewness of nickel in aluminium oxide.The shortcoming of the method is that precipitation temperature is higher, and the ammonia discharged in precipitation process also result in environmental pollution.
Summary of the invention
In order to overcome weak point of the prior art, the invention provides a kind of preparation method of nickel-base hydrogenation catalyst.The method non-environmental-pollution, in gained catalyst, active metal nickel is evenly distributed on catalyst support surface, improves the utilization rate of active metal, and then improves the activity of catalyst.
The preparation method of nickel-base hydrogenation catalyst of the present invention, comprising:
(1) the predecessor soluble-salt of active component nickel and the predecessor soluble-salt of auxiliary agent are dissolved in water, be made into nickeliferous and mixed aqueous solution that is auxiliary agent, then by as carrier aluminium oxide or/and silica add nickeliferous and and auxiliary agent mixed aqueous solution in form slurries;
(2) by the Alkali Soluble salt wiring solution-forming as precipitating reagent;
(3) water purification is added in a kettle., start and stir and reactor is heated, when temperature of reaction kettle reaches reaction temperature, and stream adds slurries that step (1) obtains and the precipitant solution that step (2) obtains, the pH value controlling slurries in reactor is 6.0 ~ 10.0;
(4) after reaction terminates, pH value to 10.0 ~ 12.0 of slurries in adjustment reactor, and leave standstill under this pH value and temperature conditions;
(5) material of step (4) gained after filtration, washing, dry, obtain nickel-base hydrogenation catalyst precursor;
(6) in the material of step (5), add peptizing agent and water purification carries out kneading, material kneading evenly after, through extruded moulding, shaping rear material drying, roasting, obtain nickel-base hydrogenation catalyst of the present invention.
The nickel-base hydrogenation catalyst of the inventive method gained, with the weight of nickel-base hydrogenation catalyst for benchmark, the content of active metal nickel is 20% ~ 70%, auxiliary agent with the content of oxide basis for 1% ~ 10.0%, be preferably 3.0% ~ 10.0%, the content of described alumina catalyst support and/or silica is 20.0% ~ 70.0%.
In step (1), the concentration of the mixed aqueous solution of described nickeliferous and auxiliary agent is 0.2 ~ 1.0mol/L.The predecessor soluble-salt of described active component nickel is one or more in nickel nitrate, nickelous sulfate, nickel chloride and nickel acetate.The nitrate that the predecessor soluble-salt of described auxiliary agent is added auxiliary agent or and/or sulfate.Described alumina catalyst support or/and silica can be in boehmite, the aluminium oxide of various crystal formation, silica, diatomite, kaolin one or more.
Described auxiliary agent is one or more in IIA race alkaline-earth metal, I B group 4 transition metal, IIB group 4 transition metal, group VIII transition metal and lanthanide series metal.In the present invention, described auxiliary agent can be selected according to processing raw material, and nickel crystallite preferably can be suppressed to increase, and improves the material of catalyst nickel reduction degree and increase catalyst sulfur resistance, as one or more in Fe, Mg, Cu, Zn, Co, La, Ce.
In step (2), described Alkali Soluble salt is one or more in NaOH, potassium hydroxide, sodium carbonate, potash, sodium acid carbonate and saleratus, and its concentration is 0.5mol/L ~ 1.5mol/L.
In step (3), the described water purification amount added in precipitation reaction still is 10% ~ 30% of step (3) gained material cumulative volume; Described reaction temperature is 60 DEG C ~ 100 DEG C; The described speed adding material in reactor is as follows: the speed that adds of step (1) gained slurries is 20mL/min ~ 80mL/min, and the speed that adds of step (2) gained alkaline sedimentation agent solution is 40mL/min ~ 100mL/min.
After reaction described in step (4) terminates, the pH value of reactor is adjusted to 10.0 ~ 12.0, temperature of reaction kettle remains on 60 DEG C ~ 100 DEG C, and time of repose is 20 minutes ~ 100 minutes;
In step (5), described washing is that when cleaning solution pH is 6.5 ~ 7.5, washing terminates with water purification washing.Described drying condition is as follows: dry 1h ~ 12h in 100 ~ 140 DEG C of drying boxes.
In step (6), described peptizing agent can be in nitric acid, acetic acid and citric acid one or more.Described catalyst can be column type, trifolium-shaped or bunge bedstraw herb type; Described drying condition is as follows: dry 1h ~ 12h in 100 DEG C ~ 140 DEG C drying boxes; Described roasting condition is: roasting 3h ~ 12h at 300 DEG C ~ 650 DEG C.
The nickel-base hydrogenation catalyst of the inventive method gained, can be used for C
5petropols, C
9petropols and C
5, C
9in blended hydrogenation of petroleum resin decolorization, can also be used for co hydrogenation (methanation), steam reformation, vaporization waits the hydrotreated lube base oil process of reaction and unsaturated hydrocarbons.
The advantage of the inventive method is: the slurries that carrier material and active component are made and alkaline precipitating agent stream adds reactor, ensure that active component homogeneous precipitation on carrier, ensure that the high uniformity dispersion of active component on carrier; Meanwhile, owing to adopting and streamedly to precipitate, also ensure that in precipitation process that to precipitate environment homogeneous, sediment is existed with same shape and grain size.The high-nickel catalyst prepared has good double bond and part benzene ring hydrogenation saturability and decolorizing effect preferably, is specially adapted to C
5petropols, C
9petropols and C
5, C
9blended hydrogenation of petroleum resin decolouring catalyst.
Accompanying drawing explanation
Fig. 1 is the XRD figure of embodiment and comparative example gained nickel-base hydrogenation catalyst.
Detailed description of the invention
Embodiment 1
279.5g six water nickel chloride, 11.0g lanthanum nitrate hexahydrate are mixed with mixed solution, make two kinds of salt be 0.6mol/L in the concentration of this solution, after two kinds of salt all dissolve, add boehmite (containing Al
2o
370% (mass fraction)) 92.9g, makes slurries stand-by, by soluble in water for 318g sodium carbonate, be mixed with the precipitant solution that concentration is 1.0mol/L, stand-by, pre-add 1000mL water purification in 8000mL reactor, heat and open mixing plant, when temperature rises to 80 DEG C, keep temperature in the kettle, start and stream adds mixed serum and alkaline sedimentation agent solution, the flow controlling mixed serum is 40mL/min and alkaline precipitating agent liquid inventory 55mL/min, the pH value keeping slurries in reactor is 7.2, after acidic mixed slurries all add, with alkaline sedimentation agent solution, slurry pH value in reactor is adjusted to 10.5, temperature now and pH value is kept to start to leave standstill, leave standstill after 30 minutes, filter and remove mother liquor, and carry out washing to remove a small amount of water-solubility impurity residual on sediment with water purification, when washings pH value is 6.5, washing terminates, filter cake is placed in 120 DEG C of drying boxes dry 3 hours.Take dry rear material 100g, add 3.0g nitric acid and 80g water purification carries out kneading, the material that kneading is good carries out extruded moulding on banded extruder, and molding materials is placed in 100 DEG C of drying boxes dry 10 hours, under 300 DEG C of conditions, roasting 10 hours, obtains nickel-base hydrogenation catalyst C
1, its analysis result is in table 1 and Fig. 1.
Embodiment 2
Preparation process with embodiment 1, just by two kinds of salt in the solution concentration be changed to 0.3mol/L, precipitant solution concentration is changed to 1.5mol/L, and the nickel-base hydrogenation catalyst of preparation is C
2, its analysis result is in table 1.
Embodiment 3
Preparation process with embodiment 1, by pre-add 1500mL water purification in 8000mL reactor, the nickel-base hydrogenation catalyst C of preparation
3, its analysis result is in table 1.
Embodiment 4
Reactor temperature, with embodiment 1, is risen to 100 DEG C by preparation process, after acidic mixed slurries all add, with alkaline sedimentation agent solution, slurry pH value in reactor is adjusted to 12; Time of repose is extended to 100 minutes, filter and remove mother liquor, and carry out washing to remove a small amount of water-solubility impurity residual on sediment with water purification, washings pH value is 7.0, prepares nickel-base hydrogenation catalyst C
4, its analysis result is in table 1 and Fig. 1.
Embodiment 5
Preparation process with embodiment 1, by and the flow that stream adds mixed serum changes 80mL/min and alkaline precipitating agent liquid inventory 100mL/min into, the pH value of slurries in reactor carried is 9.5 simultaneously, prepares nickel-base hydrogenation catalyst C
5, its analysis result is in table 1.
Embodiment 6
Boehmite, with embodiment 1, is changed into 65g γ-Al by preparation process
2o
3(being greater than 150 order powder), make slurries; Prepare nickel-base hydrogenation catalyst C
6, its analysis result is in table 1.
Embodiment 7
Preparation process is with embodiment 1, mixed solution is made up of 290.8g six water nickel nitrate and 59.4g zinc nitrate and 29.1g copper nitrate, mixed solution concentration 1.0mol/L, boehmite is changed to 65g silicon-dioxide powdery (being greater than 150 order powder), precipitating reagent sodium carbonate liquor changes the sodium hydroxide solution of 1.0mol/L concentration into, obtained nickel-base hydrogenation catalyst C
7, analysis result is in table 1 and Fig. 1.
Embodiment 8
Preparation process is with embodiment 1, mixed solution is made up of 290.8g six water nickel nitrate and 59.4g zinc nitrate and 29.1g copper nitrate, mixed solution concentration 1.0mol/L, boehmite is changed to 50g diatomite powder (being greater than 150 order powder), precipitating reagent sodium carbonate liquor changes sodium carbonate and the potash mixed solution of 1.0mol/L concentration into, obtained nickel-base hydrogenation catalyst C
8, analysis result is in table 1.
Embodiment 9
Preparation process with embodiment 1, by boehmite (containing Al
2o
370% (mass fraction)) addition carries to 363.5g, prepares nickel-base hydrogenation catalyst C
9, its analysis result is in table 1 and Fig. 1.
Embodiment 10
Preparation process with embodiment 1, by boehmite (containing Al
2o
370% (mass fraction)) addition is down to 11.3g, prepares nickel-base hydrogenation catalyst C
10, its analysis result is in table 1 and Fig. 1.
Embodiment 11
Peptizing agent in forming process, with embodiment 1, is changed into 6g acetic acid and 10g citric acid mixed solution, prepares nickel-base hydrogenation catalyst C by preparation process
11.Its analysis result is in table 1.
Embodiment 12
Preparation process, with embodiment 1, by molding materials at temperature 140 DEG C dry 5 hours, and roasting 4 hours at 650 DEG C, prepares nickel-base hydrogenation catalyst C
12.Its analysis result is in table 1 and Fig. 1.
Comparative example
Nickel-base hydrogenation catalyst is prepared by CN200610016260.3.
By soluble in water for 318g sodium carbonate, being mixed with concentration is that the precipitant solution of 1.0mol/L puts into reactor, when being heated to 70 DEG C, keeps temperature in the kettle.279.5g six water nickel chloride is mixed with the solution that concentration is 0.6mol/L, joins in the sodium carbonate liquor in still and precipitate, until solution containing nickel precipitates completely.Precipitation end adds solid alumina 65g, stirs after 0.5-1.0 hour and washs, and filter cake is placed in 120 DEG C of drying boxes dry 3 hours.Take dry rear material 100g, add 3.0g nitric acid and 80g water purification carries out kneading, the material that kneading is good carries out extruded moulding on banded extruder, molding materials is placed in 120 DEG C of drying boxes dry 3 hours, roasting 10 hours under 300 DEG C of conditions, obtain nickel-base hydrogenation catalyst B, its analysis result is in table 1 and Fig. 1.
The physico-chemical property of the nickel-base hydrogenation catalyst of table 1 embodiment and comparative example gained
| Catalyst | C 1 | C 2 | C 3 | C 4 | C 5 | C 6 | C 7 | C 8 | C 9 | C 10 | C 11 | C 12 | B |
| Ni，％ | 37.5 | 36.8 | 38.2 | 37.9 | 38.1 | 44.1 | 34.2 | 37.8 | 20.1 | 69.3 | 38.2 | 37.2 | 32.1 |
| Al 2O 3，％ | 50.2 | 50.3 | 51.9 | 50.8 | 50.9 | 41.3 | 19.8 | 73.4 | 7.9 | 49.3 | 50.8 | 58.1 | |
| SiO 2，％ | - | - | - | - | - | - | 40.5 | 31.3 | - | - | - | - | - |
| La 2O 3，％ | 2.20 | 2.19 | 2.28 | 2.25 | 2.21 | 2.61 | 1.2 | 4.1 | 2.18 | 2.24 | - | ||
| ZnO，％ | - | - | - | - | - | - | 10.1 | 11.0 | - | - | - | - | - |
| CuO，％ | - | - | - | - | - | - | 6.1 | 6.6 | - | - | - | - | |
| Pore volume, mL/g | 0.413 | 0.425 | 0.401 | 0.418 | 0.409 | 0.415 | 0.438 | 0.404 | 0.442 | 0.386 | 0.420 | 0.421 | 0.368 |
| Specific surface, m 2/g | 187 | 194 | 168 | 186 | 176 | 188 | 175 | 205 | 209 | 226 | 192 | 169 | 167 |
Note: the percentage in table 1 is mass fraction
Choose the catalyst C of preparation
1, C
4, C
8, C
12and B evaluates on miniature fixed bed hydrogenation reaction unit, this device has two tandem reactors, and each reactor catalyst loading amount is 10mL, catalyst is before hydrogenation reaction, and with hydrogen reducing, reducing condition is as follows: temperature 380 DEG C, hydrogen dividing potential drop 6MPa, hydrogen volume air speed is 600h
-1, the recovery time is 6 hours.C is dissolved with cyclohexane
9petropols are raw material, and the Petropols ratio accounted in raw material is 10% ~ 50% (mass fraction), and after hydrogenation, product obtains hydrogenated petroleum resin after distillation removing cyclohexane.Petropols character and appreciation condition are in table 2 and table 3, and the product index of each embodiment is in table 4.
Table 2 Petropols feedstock property
| Resin softening point/DEG C | 118 |
| Color (Sai Shi) | 4 # |
| S/μg·g -1 | 130 |
| Bromine valency/gBr100mL -1 | 24.14 |
Table 3 evaluating catalyst process conditions
| Reaction pressure/MPa | 8.0 |
| Volume space velocity (relative to Petropols)/h -1 | 0.6 |
| Hydrogen to oil volume ratio (relative to Petropols) | 1000 |
| Reaction temperature/DEG C | 265 |
The evaluation result of table 4 catalyst
| Catalyst | C 1 | C 4 | C 8 | C 12 | B |
| Hydrogenation resin softening point/DEG C | 112 | 112 | 111 | 113 | 109 |
| Form and aspect | Water white | Water white | Water white | Water white | Water white |
| S/μg·g -1 | 0.53 | 0.58 | 0.42 | 0.55 | 0.55 |
| Bromine valency/gBr100mL -1 | 0.966 | 0.869 | 0.724 | 1.09 | 1.69 |
| Double bond conversion rate/% (mass fraction) | 96.0 | 96.4 | 97.0 | 95.5 | 93.0 |
Note:
Claims (14)
1. a preparation method for nickel-base hydrogenation catalyst, comprising:
(1) the predecessor soluble-salt of active component nickel and the predecessor soluble-salt of auxiliary agent are dissolved in water, be made into nickeliferous and mixed aqueous solution that is auxiliary agent, then using as carrier aluminium oxide or/and silica add nickeliferous and and auxiliary agent mixed aqueous solution in form slurries;
(2) using the Alkali Soluble salt wiring solution-forming as precipitating reagent;
(3) water purification is added in a kettle., start and stir and reactor is heated, when temperature of reaction kettle reaches reaction temperature, and stream adds slurries that step (1) obtains and the precipitant solution that step (2) obtains, the pH value controlling slurries in reactor is 6.0 ~ 10.0; Described reaction temperature is 60 DEG C ~ 100 DEG C;
(4) after reaction terminates, pH value to 10.5 ~ 12.0 of slurries in adjustment reactor, and leave standstill under this pH value and temperature conditions;
(5) material of step (4) gained after filtration, washing, dry, obtain nickel-base hydrogenation catalyst precursor;
(6) in the material of step (5), add peptizing agent and water purification carries out kneading, material kneading evenly after, through extruded moulding, shaping rear material drying, roasting, obtain nickel-base hydrogenation catalyst; With the weight of nickel-base hydrogenation catalyst for benchmark, the content of active metal nickel is 20% ~ 70%, and auxiliary agent is with the content of oxide basis for 1% ~ 10.0%, and the content of described alumina catalyst support and/or silica is 20.0% ~ 70.0%.
2. in accordance with the method for claim 1, it is characterized in that described auxiliary agent is one or more in II race alkaline-earth metal, I B group 4 transition metal, II B group 4 transition metal, group VIII transition metal and lanthanide series metal.
3. in accordance with the method for claim 1, it is characterized in that described auxiliary agent is one or more in Fe, Mg, Cu, Zn, Co, La, Ce.
4. in accordance with the method for claim 1, it is characterized in that described auxiliary agent with the weight content of oxide basis in nickel-base hydrogenation catalyst for 3.0% ~ 10.0%.
5. in accordance with the method for claim 1, it is characterized in that the predecessor soluble-salt of described active component nickel is one or more in nickel nitrate, nickelous sulfate, nickel chloride and nickel acetate; The nitrate that the predecessor soluble-salt of described auxiliary agent is added auxiliary agent or and/or sulfate.
6. the concentration that in accordance with the method for claim 1, it is characterized in that the mixed aqueous solution of described nickeliferous and auxiliary agent is 0.2 ~ 1.0mol/L.
7. in accordance with the method for claim 1, it is characterized in that described alumina catalyst support or/and silica is one or more in boehmite, the aluminium oxide of various crystal formation, silica, diatomite, kaolin.
8. in accordance with the method for claim 1, it is characterized in that in step (2), described Alkali Soluble salt is one or more in NaOH, potassium hydroxide, sodium carbonate, potash, sodium acid carbonate and saleratus, and its concentration is 0.5mol/L ~ 1.5mol/L.
9. in accordance with the method for claim 1, it is characterized in that in step (3), the water purification amount added in reactor is 10% ~ 30% of step (3) gained material cumulative volume.
10. in accordance with the method for claim 1, it is characterized in that in step (3), the speed adding material in reactor is: the speed that adds of step (1) gained slurries is 20mL/min ~ 80mL/min, and the speed that adds of step (2) gained alkaline sedimentation agent solution is 40mL/min ~ 100mL/min.
11. in accordance with the method for claim 1, and it is characterized in that in step (4), is 10.5 ~ 12.0 in pH value, and under temperature of reaction kettle 60 DEG C ~ 100 DEG C conditions, time of repose is 20 minutes ~ 100 minutes.
12. in accordance with the method for claim 1, it is characterized in that in step (5), and described washing is that when cleaning solution pH is 6.5 ~ 7.5, washing terminates with water purification washing.
13. in accordance with the method for claim 1, it is characterized in that in step (5), described drying condition is as follows: at 100 ~ 140 DEG C of dry 1h ~ 12h.
14. in accordance with the method for claim 1, it is characterized in that in step (6), described drying condition is as follows: at 100 DEG C ~ 140 DEG C dry 1h ~ 12h; Described roasting condition is: roasting 3h ~ 12h at 300 DEG C ~ 650 DEG C.
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