CN105061155B - A kind of method for preparing 3,5 xylenols - Google Patents
A kind of method for preparing 3,5 xylenols Download PDFInfo
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- CN105061155B CN105061155B CN201510434001.1A CN201510434001A CN105061155B CN 105061155 B CN105061155 B CN 105061155B CN 201510434001 A CN201510434001 A CN 201510434001A CN 105061155 B CN105061155 B CN 105061155B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/06—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by conversion of non-aromatic six-membered rings or of such rings formed in situ into aromatic six-membered rings, e.g. by dehydrogenation
- C07C37/07—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by conversion of non-aromatic six-membered rings or of such rings formed in situ into aromatic six-membered rings, e.g. by dehydrogenation with simultaneous reduction of C=O group in that ring
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/86—Chromium
- B01J23/866—Nickel and chromium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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Abstract
A kind of method that mixed oxide catalyst catalysis isophorone aromatization prepares 3,5 xylenols, it is related to the method for the xylenol of preparation 3,5.Method：First, iron nickel chromium triangle mixed oxide catalyst is sieved；2nd, the iron nickel chromium triangle oxide after isophorone and shaping and roasting is subjected to aromatization, that is, completed.Iron nickel chromium triangle oxide used of the invention is synthesized using precipitation hydro-thermal method or conventional sol gel method, iron nickel chromium triangle mixed oxide is catalyzed the aromatization of isophorone, the reaction that overcomes the presence of the homogeneous catalysts such as iodomethane is discontinuous, difficult, equipment corrosion is separated with product seriously and the drawback such as environmental pollution, with higher reactivity and 3, the selectivity of 5 xylenols and higher carbon accumulation resisting ability；Reaction product and catalyst are easily separated in the present invention；It is simple to operate, it is easy to large-scale production.
Description
Technical field
The present invention relates to a kind of method for preparing MX, and in particular to a kind of iron nickel chromium triangle mixed oxide is urged
The method that agent catalysis isophorone aromatisation prepares MX.
Background technology
MX is important Industrial intermediates, mainly for the preparation of antioxidant, antibiotic, resin-bonding
The production of agent and vitamin E etc., is also widely used for various antibacterials, mould proof processing procedure, such as leather, paper, textile and photograph
The antibacterial and mouldproof processing of piece etc..The world today increasingly increases the demand of MX, and the annual yield in the whole world
Fewer, domestic yield is less, it is difficult to meet the demand in market.At present, the method for domestic production MX
It is meta-xylene sulfonation alkali solution technique, the complex technical process is seriously polluted, and product purity is not high.It is different compared with conventional method
Phorone aromatisation one-step method prepares MX, can cause atom utilization up to 88.39%, much larger than Traditional Method
Preparation technology, and product is single, is easily purified, and is a kind of environmental protection suddenly technique leaved for development.
Early in the 1940s, it is 668-676 DEG C of bar to be reported first in United States Patent (USP) with isophorone in temperature
Under part, to prepare MX.But due to not using catalyst at that time, therefore yield is relatively low.Later by research,
Start to use homogeneous catalyst, used homogeneous catalyst is the aliphatic hydrocarbon or aromatic hydrocarbon being substituted with halogen atoms, but is used
The catalyst has catalyst and difficulty is separated with reaction product, the problems such as reacting discontinuous, therefore, and multiphase is studied at this stage and is urged
Agent becomes focus.Up to now, successively someone has used V205/A1203、Mo03/Al2O3, rare-earth oxide (rubidium praseodymium
Mixed oxide) and Cr203/A1203It is used for Deng multiple catalysts in the reaction that isophorone prepares 3,5 one xylenols,
But it is fast to there is inactivation, the low problem of selectivity.At present, iron-nickel-chromium can solve Catalysts Deactivation Problems, but it is transported
The row time is only capable of maintaining 135h, and selectivity of product is relatively low, and Catalyst Production cost is higher.At present, without a kind of heterogeneous catalysis
Agent can realize the report of the continuous running of reaction under conditions of selectivity of product is ensured, we will precipitate hydro-thermal or molten first
Multi-component oxide prepared by sol-gel applies to this reaction, it is possible to achieve selectivity of product is realized instead under conditions of higher
The continuous running answered, it is possible to achieve the large-scale production of product.
The content of the invention
3,5- dimethyl is prepared it is an object of the present invention to provide a kind of iron nickel chromium triangle mixed oxide catalysis isophorone aromatisation
The method of phenol, is realized according to the following steps：
A kind of method for preparing MX, is comprised the following steps that：
1) catalyst loads the flat-temperature zone of fixed-bed micro-reactor stainless steel reaction pipe；
2) isophorone is continuously injected into the beds of fixed-bed micro-reactor using measuring pump, entered with catalyst
Row aromatization, reaction temperature is 450-600 DEG C, and pressure is 1.5-5MPa, and mass space velocity is 0.5-2h-1, nitrogen flow rate is
20-60ml/min, reaction time 5h, that is, obtain MX；
Described catalyst is the iron nickel chromium triangle mixed oxide of 20-40 mesh.
It is preferred that, step 2) described in reaction temperature be 570 DEG C, pressure is 2.5MPa, and mass space velocity is 1h-1, nitrogen
Flow velocity is 40ml/min.
The preparation method of described iron nickel chromium triangle mixed oxide, is comprised the following steps that：
1) 1 part of six water nickel nitrate, 2~4 parts of nine water chromic nitrate, 8~16 parts of nine water ferric nitrate, deionization are weighed by weight
10~18 parts of water；
2)a:By step 1) the six water nickel nitrates, nine water chromic nitrates, the nine water ferric nitrates that have weighed are added in deionized water,
Room temperature low whipping speed is 10~50min of stirring under conditions of 300~500r/min, dissolves it, makes solution A；b:
Mixing speed is under conditions of 300~700r/min, surfactant is added in solution A prepared by step a, after adding,
Mixed solution B is made to be stirred 1 hour under conditions of 100~300r/min in low whipping speed again；
3) to step 2) obtained by B solution in add precipitating reagent, control 20~80 DEG C of temperature, regulation pH value is 8-11, is put
In the closed reactor of the stainless steel with polytetrafluoroethyllining lining pad, under 100~185 DEG C of temperature conditionss crystallization 3~
24h, is cooled to 25 DEG C, through centrifuging, filtering, be washed with deionized, dry after obtain mixed oxide；
4) to step 3) obtained by mixed oxide in add adhesive, product is made in tabletting, 550 DEG C of roastings；
Described step 2) in added surfactant be selected from cetyl trimethylammonium bromide, Macrogol 6000,
One kind in neopelex, polyvinylpyrrolidone, and consumption is the 1%~5% of solid mixture gross weight；
Described step 3) in one kind in urea, ammoniacal liquor of precipitating reagent；The mass fraction of described ammoniacal liquor is
25%.
Described step 4) in one kind in polyacrylamide, aluminum oxide of adhesive, and consumption is solid mixing
The 1%~5% of thing gross weight.
The process for preparing 3,5 1 xylenols by isophorone is divided into two parts：A part is absorption in catalyst
Isophorone demethanation process on surface；Another part is that the isophorone for sloughing methane carries out the rearrangement of the phenol of dienone one, shape
Into 3,5 1 xylenols, the absorption by catalyst surface metal to carbonylic oxygen atom so that towering key pine in C=O bond
Relax, towering electronics is shifted to metal direction.The towering key in C=O bond is occurred covalent bond heterolytic fission, form carbonium ion.Together
When, in isophorone molecule, because methylene carbon is joined directly together with carbonylic carbon atom, the δ keys of C=O bond and α-C-H
Produce to surpass and grip effect altogether, the result of electron delocalization influence makes C-H δ keys polarize, and hydrogen atom shows certain acidity.Separately
Outside, the carbon atom of methylene is Sp3 hydridization, and the carbonylic carbon atom of it and Sp2 hydridization is joined directly together, due to sp2 hydbridized carbon atoms
There is stronger electronegativity than sp3 hydbridized carbon atoms, the result of inductive effect influence makes hydrogen atom have certain activity, due to super
The result of effect and inductive effect influence is gripped altogether, and hydrogen atom is very active, and shows certain acidity, can adsorb and urge
On the oxygen atom on agent surface, methylene carbon then forms carbanion, because resonance effects electronics is shifted,
So that the carbon on five forms carbanion, this allows for the carbon-carbon bond reduction that it is connected with methyl.Under high temperature action, carbon
δ keys fracture between anion and methine carbon atom.Hydrogen of the methyl taken off with absorption on catalyst surface is combined, and forms first
Alkane molecule, while isophorone also becomes dienone, due to resonant interaction, carbonium ion is shifted, and forms 3,5- diformazans
The resonance hybrid of base phenol, ultimately forms MX.
Iron and nickel have a resistance to deactivation, and chromium oxide wherein O2-For basic center, dehydrogenation, Cr are played3+For in acid
The heart, plays aromatisation, is to be applied to a kind of relatively more extensive activated centre of dehydroaromatizationof at present.It is this multiple that we synthesize
Close oxide catalyst and be different from the catalyst of mechanical mixture, oxonium ion closs packing in a certain way, metal cation by its from
Sub- radius size is filled in by O2-On the suitable clearance position of composition, independent oxygen-containing acid ion is not present in structure.This is just
So that the decentralization of this several metal is higher, at present, the biggest problem for being catalyzed this reaction is the carbon distribution problem of catalyst.This is several
Synergy between metal solves the problems, such as the carbon distribution of catalyst while higher conversion is ensured with selectivity.After product
Continuous lock out operation is simple, and this technique is easily achieved industrialization.
The advantage of the invention is that：
1st, mixed oxide catalyst of the present invention, is prepared using precipitation hydro-thermal or sol-gal process, simple easy
OK.
2nd, production technology of the present invention synthesizes MX using one-step method multiphase successive reaction, pollutes small, product
It is easily separated with catalyst.
3rd, institute's invention catalyst is applied to be catalyzed the technique, with long-play, can reduce the filling frequency of catalyst,
The material consumption for stopping work and energy consumption are reduced, the large-scale production of product is easily realized.
Brief description of the drawings
Fig. 1 is isophorone conversion ratio and the graph of relation in reaction time.
Embodiment
Technical solution of the present invention is not limited to act embodiment set forth below, in addition to any between each specific implementation
Combination.
Embodiment 1
First, the iron nickel chromium triangle mixed oxide catalyst of 20-40 mesh is loaded into fixed-bed micro-reactor stainless steel reaction pipe
Flat-temperature zone.
The 2nd, raw material isophorone is continuously injected into the beds of fixed-bed micro-reactor using measuring pump, with iron
Nickel chromium triangle mixed oxide catalyst carries out aromatization, and reaction temperature is 450 DEG C, and pressure is 1.5MPa, and mass space velocity is
0.5h-1, nitrogen flow rate is 20ml/min, reaction time 5h, that is, completes iron nickel chromium triangle mixed oxide catalysis isophorone aromatisation
Prepare 3,5- xylenols；
The mixed oxide catalyst of iron nickel chromium triangle described in the present embodiment is using co-precipitation hydro-thermal method synthesis, specific synthesis side
Method is as follows：Nine water ferric nitrates, six water nickel nitrates, nine water chromic nitrates are pressed into iron oxide：Chromium oxide：Nickel oxide=8.69:1.15:1
Ratio of weight and number dissolving, add 5% oxide weight fraction cetyl trimethylammonium bromide, add ammoniacal liquor regulation pH value
To 10, crystallization 12h in 180 DEG C of baking ovens is placed in after stirring, it is scrubbed, be dried to obtain mixed oxide, add 3% weight
It is made after the aluminum oxide of fraction, compression molding, 550 DEG C of roasting 3h.
The time that the first drop product will be flowed out in the present embodiment is calculated as the t=0 moment, and gathers a product per each 5h, uses
Gas-chromatography is analyzed, and conversion ratio, the yield of MX, reaction time of isophorone are calculated with internal standard method
1 is the results are shown in Table during 200h.
Table 1
Embodiment 2
First, the iron nickel chromium triangle mixed oxide catalyst of 20-40 mesh is loaded into fixed-bed micro-reactor stainless steel reaction pipe
Flat-temperature zone.
The 2nd, raw material isophorone is continuously injected into the beds of fixed-bed micro-reactor using measuring pump, with iron
Nickel chromium triangle mixed oxide catalyst carries out aromatization, and reaction temperature is 600 DEG C, and pressure is 5MPa, and mass space velocity is 2h-1,
Nitrogen flow rate is 60ml/min, reaction time 5h, that is, completes iron nickel chromium triangle mixed oxide catalysis isophorone aromatisation and prepare 3,
5- xylenols；
The mixed oxide catalyst of iron nickel chromium triangle described in the present embodiment is using co-precipitation hydro-thermal method synthesis, specific synthesis side
Method is as follows：Nine water ferric nitrates, six water nickel nitrates, nine water chromic nitrates are pressed into iron oxide：Chromium oxide：Nickel oxide=10.05:2.59:1
Ratio of weight and number dissolving, add 3% oxide weight fraction Macrogol 6000, add mass fraction be 25% ammoniacal liquor
PH value is adjusted to 10, crystalline substance China 12h in 180 DEG C of baking ovens is placed in after stirring, scrubbed, be dried to obtain mixed oxide, addition
It is made after the polyacrylamide of 3% weight fraction, compression molding, 550 DEG C of roasting 3h.
The time that the first drop product will be flowed out in the present embodiment is calculated as the t=0 moment, and gathers a product per each 5h, uses
Gas-chromatography is analyzed, and conversion ratio, the yield of MX, reaction time of isophorone are calculated with internal standard method
2 are the results are shown in Table during 5h.
Table 2
Embodiment 3
First, the iron nickel chromium triangle mixed oxide catalyst of 20-40 mesh is loaded into fixed-bed micro-reactor stainless steel reaction pipe
Flat-temperature zone.
The 2nd, raw material isophorone is continuously injected into the beds of fixed-bed micro-reactor using measuring pump, with iron
Nickel chromium triangle mixed oxide catalyst carries out aromatization, and reaction temperature is 570 DEG C, and pressure is 2.5MPa, and mass space velocity is 1h-1, nitrogen flow rate is 40ml/min, reaction time 5h, that is, completes iron nickel chromium triangle mixed oxide catalysis isophorone aromatisation and prepare
3,5- xylenols；
The mixed oxide catalyst of iron nickel chromium triangle described in the present embodiment is using co-precipitation hydro-thermal method synthesis, specific synthesis side
Method is as follows：Nine water ferric nitrates, six water nickel nitrates, nine water chromic nitrates are pressed into iron oxide：Chromium oxide：Nickel oxide=9.62:2.74:1
Ratio of weight and number dissolving, add the neopelex of 2% oxide weight fraction, it is 25% to add mass fraction
Ammoniacal liquor adjusts pH value to 10, is placed in crystalline substance China 12h in 180 DEG C of baking ovens after stirring, scrubbed, be dried to obtain mixed oxide,
It is made after adding the aluminum oxide of 4% weight fraction, compression molding, 550 DEG C of roasting 3h.
The time that the first drop product will be flowed out in the present embodiment is calculated as the t=0 moment, and gathers a product per each 5h, uses
Gas-chromatography is analyzed, and conversion ratio, the yield of MX, reaction time of isophorone are calculated with internal standard method
3 are the results are shown in Table during 5h.
Table 3
Embodiment 4
First, the iron nickel chromium triangle mixed oxide catalyst of 20-40 mesh is loaded into fixed-bed micro-reactor stainless steel reaction pipe
Flat-temperature zone.
The 2nd, raw material isophorone is continuously injected into the beds of fixed-bed micro-reactor using measuring pump, with iron
Nickel chromium triangle mixed oxide catalyst carries out aromatization, and reaction temperature is 500 DEG C, and pressure is 3.0MPa, and mass space velocity is
1.5h-1, nitrogen flow rate is 40ml/min, reaction time 5h, that is, completes iron nickel chromium triangle mixed oxide catalysis isophorone aromatisation
Prepare 3,5- xylenols；
The mixed oxide catalyst of iron nickel chromium triangle described in the present embodiment is using co-precipitation hydro-thermal method synthesis, specific synthesis side
Method is as follows：Iron chloride, six water nickel nitrates, nine water chromic nitrates are pressed into iron oxide：Nickel oxide：Chromium oxide=15.62:1:2.74 weight
Portion rate dissolving is measured, the polyvinylpyrrolidone of 4% oxide weight fraction is added, ammoniacal liquor is added and adjusts pH value to 10, stirring
It is placed in crystalline substance China 12h in 180 DEG C of baking ovens after uniform, it is scrubbed, be dried to obtain mixed oxide, the oxidation of 5% weight fraction of addition
It is made after aluminium, compression molding, 550 DEG C of roasting 3h.
The time that the first drop product will be flowed out in the present embodiment is calculated as the t=0 moment, and gathers a product per each 5h, uses
Gas-chromatography is analyzed, and conversion ratio, the yield of MX, reaction time of isophorone are calculated with internal standard method
4 are the results are shown in Table during 200h.
Table 4
Embodiment 5
First, the iron nickel chromium triangle mixed oxide catalyst of 20-40 mesh is loaded into fixed-bed micro-reactor stainless steel reaction pipe
Flat-temperature zone.
The 2nd, raw material isophorone is continuously injected into the beds of fixed-bed micro-reactor using measuring pump, with iron
Nickel chromium triangle mixed oxide catalyst carries out aromatization, and reaction temperature is 560 DEG C, and pressure is 2.7MPa, and mass space velocity is
1.5h-1, nitrogen flow rate is 50ml/min, reaction time 5h, that is, completes iron nickel chromium triangle mixed oxide catalysis isophorone aromatisation
Prepare 3,5- xylenols；
The mixed oxide catalyst of iron nickel chromium triangle described in the present embodiment is using co-precipitation hydro-thermal method synthesis, specific synthesis side
Method is as follows：Nine water ferric nitrates, six water nickel nitrates, nine water chromic nitrates are pressed into iron oxide：Nickel oxide：Chromium oxide=14.60:2.30:1
Ratio of weight and number dissolving, add 5% oxide weight fraction cetyl trimethylammonium bromide, add urea regulation pH value
To 10, crystallization 12h in 180 DEG C of baking ovens is placed in after stirring, it is scrubbed, be dried to obtain mixed oxide, add 3% weight point
It is made after several polyacrylamides, compression molding, 550 DEG C of roasting 3h.
The time that the first drop product will be flowed out in the present embodiment is calculated as the t=0 moment, and gathers a product per each 5h, uses
Gas-chromatography is analyzed, and conversion ratio, the yield of MX, reaction time of isophorone are calculated with internal standard method
5 are the results are shown in Table during 200h.
Table 5
Embodiment 6
First, the iron nickel chromium triangle mixed oxide catalyst of 20-40 mesh is loaded into fixed-bed micro-reactor stainless steel reaction pipe
Flat-temperature zone.
The 2nd, raw material isophorone is continuously injected into the beds of fixed-bed micro-reactor using measuring pump, with iron
Nickel chromium triangle mixed oxide catalyst carries out aromatization, and reaction temperature is 590 DEG C, and pressure is 4.5MPa, and mass space velocity is
1.7h-1, nitrogen flow rate is 55ml/min, reaction time 5h, that is, completes iron nickel chromium triangle mixed oxide catalysis isophorone aromatisation
Prepare 3,5- xylenols；
The mixed oxide catalyst of iron nickel chromium triangle described in the present embodiment is using sol-gal process synthesis, specific synthetic method
It is as follows：Nine water ferric nitrates, six water nickel nitrates, nine water chromic nitrates are pressed into iron oxide：Nickel oxide：Chromium oxide=9.60:2.30:1
Ratio of weight and number dissolve, add 5% oxide weight fraction cetyl trimethylammonium bromide, add urea adjust pH value to
10, expansion curing in 180 DEG C of baking ovens is positioned over, crystallization 12h in 180 DEG C of baking ovens is placed in after stirring, it is scrubbed, be dried to obtain
Mixed oxide, is made after adding the polyacrylamide of 3% weight fraction, compression molding, 550 DEG C of roasting 3h.
The time that the first drop product will be flowed out in the present embodiment is calculated as the t=0 moment, and gathers a product per each 5h, uses
Gas-chromatography is analyzed, and conversion ratio, the yield of MX, reaction time of isophorone are calculated with internal standard method
6 are the results are shown in Table during 200h.
Table 6
Example one is used for catalyst, long period evaluation is carried out, the stability of catalyst is investigated, as seen from the figure, catalysis
Preferably, after operation 350h, isophorone conversion ratio remains to maintain 85% or so the stability of agent.
Claims (3)
1. a kind of method for preparing MX, it is characterised in that comprise the following steps that：
1. catalyst loads the flat-temperature zone of fixed-bed micro-reactor stainless steel reaction pipe；
2. isophorone is continuously injected into the beds of fixed-bed micro-reactor using measuring pump, virtue is carried out with catalyst
Structureization is reacted, and reaction temperature is 450-600 DEG C, and pressure is 1.5-5MPa, and mass space velocity is 0.5-2h-1, nitrogen flow rate is 20-
60ml/min, reaction time 5h, that is, obtain MX；
Described catalyst is the iron nickel chromium triangle mixed oxide of 20-40 mesh；
The preparation method of described iron nickel chromium triangle mixed oxide, is comprised the following steps that：
1) 1 part of six water nickel nitrate, 2~4 parts of nine water chromic nitrate, 8~16 parts of nine water ferric nitrate, deionized water 10 are weighed by weight
~18 parts；
2)a:By step 1) the six water nickel nitrates, nine water chromic nitrates, the nine water ferric nitrates that have weighed are added in deionized water, room temperature
Lower low whipping speed is 10~50min of stirring under conditions of 300~500r/min, dissolves it, makes solution A；b:Stirring
Speed is mixed under conditions of 300~700r/min, surfactant is added in solution A prepared by step a, after adding, then
Mixed solution B is made to be stirred 1 hour under conditions of 100~300r/min in low whipping speed；
3) to step 2) obtained by B solution in add precipitating reagent, control 20~80 DEG C of temperature, regulation pH value is 8-11, is placed in band
Have in the closed reactor of stainless steel of polytetrafluoroethyllining lining pad, 3~24h of crystallization under 100~185 DEG C of temperature conditionss,
Be cooled to 25 DEG C, through centrifuging, filtering, be washed with deionized, dry after obtain mixed oxide；
4) to step 3) obtained by mixed oxide in add adhesive, product is made after 550 DEG C of roastings in tabletting；
Described step 2) in added surfactant be selected from cetyl trimethylammonium bromide, Macrogol 6000,12
One kind in sodium alkyl benzene sulfonate, polyvinylpyrrolidone, and consumption is six water nickel nitrates, nine water chromic nitrates, nine water ferric nitrates
The 1%~5% of correspondence oxide solid total weight of the mixture；
Described step 3) in one kind in urea, ammoniacal liquor of precipitating reagent；
Described step 4) in one kind in polyacrylamide, aluminum oxide of adhesive, and consumption is that mixed oxide is total
The 1%~5% of weight.
2. the as claimed in claim 1 method for preparing MX, it is characterised in that step 2. described in reaction
Temperature is 570 DEG C, and pressure is 2.5MPa, and mass space velocity is 1h-1, nitrogen flow rate is 40ml/min.
3. the method as claimed in claim 1 for preparing MX, it is characterised in that the quality of described ammoniacal liquor point
Number is 25%.
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