CN104888814A - Low-temperature high-activity composite solid acid catalyst and preparation method thereof - Google Patents

Abstract

The invention discloses a low-temperature high-activity composite solid acid catalyst. The low-temperature high-activity composite solid acid catalyst is prepared from following raw materials, by weight, 48 to 55 parts of beta-aluminum oxide, 4 to 6 parts of vermiculite, 6 to 9 parts of antimonous oxide, 20 to 24 parts of silicon dioxide, 14 to 17 parts of polypropylene short fiber, 2 to 4 parts of potassium hydrogen sulfate, 10 to 13 parts of tetrabutyl titanate, 8 to 14 parts of sesbania powder, and an appropriate amount of water. The low-temperature high-activity composite solid acid catalyst is capable of solving a common failing of common metallic oxide solid acid catalysts that deactivation is easily caused; and at the same time, acid density is increased, acid strength is increased greatly, catalytic effect is excellent, and the low-temperature high-activity composite solid acid catalyst can be recycled, and is friendly to the environment.

Description

A kind of low temperature high activity composite solid-acid catalyst and preparation method thereof

Technical field

The present invention relates to solid acid catalyst technical field, be specifically related to a kind of low temperature high activity composite solid-acid catalyst and preparation method thereof.

Background technology

Ether has extensive use, and chemical industry aspect is mainly used as the fine solvent of oils, dyestuff, alkaloid, fat, resin, nitrocellulose, hydrocarbon, linseed oil, rosin fat, spices, unvulcanized rubber etc.; Medical industry is used as extractant that medicine produces and anesthetic medically; Wool spinning, cotton industry are used as greasy dirt purificant; Also can be used for gunpowder industry and manufacture cordite, its preparation method is industrial under acid catalysis, can be obtained by ethanol dehydration.

Produce in the chemical production processes of reality at present ether great majority still adopt liquid acid such as the concentrated sulfuric acid as catalyst, although have inexpensive, reaction temperature is low, conversion ratio is high, reactivity advantages of higher, but there is, raffinate serious to equipment corrosion and waste water environmental pollution is serious, operating condition is harsh, product post processing is more difficult, accessory substance is many, poor selectivity and be difficult to realize the shortcomings such as continuous seepage in technique, the needs of current environmental protection and economic development can not be met; Though existing fraction enterprise adopts solid acid catalyst aluminium oxide or molecular sieve etc. in prior art, exist be easy to solution-off, less stable, life-span compared with short, easy in inactivation, the defect such as acid strength distribution is wide, aperture is little, the surface nature of easy carbon distribution, catalyst is complicated.If prepare nontoxic composite solid-acid catalyst, then above-mentioned problems just can be resolved, and replace liquid acid as catalyst to be also the important channel realizing environmental friendly catalysis new technology with solid acid.

Summary of the invention

Object of the present invention is just to provide a kind of low temperature high activity composite solid-acid catalyst and preparation method thereof, to overcome the deficiencies in the prior art.

The object of the present invention is achieved like this:

A kind of low temperature high activity composite solid-acid catalyst, it is characterized in that, be made up of the raw material of following weight portion: beta-alumina 48-55, vermiculite 4-6, antimony oxide 6-9, silica 20-24, polypropene staple 14-17, potassium acid sulfate 2-4, butyl titanate 10-13, sesbania powder 8-14, suitable quantity of water.

The preparation method of described a kind of low temperature high activity composite solid-acid catalyst, is characterized in that comprising the following steps:

(1) potassium acid sulfate is added water to be stirred to dissolve completely, add vermiculite and soak 10-12 hour, grinding pulping, add silica and flood absorption 2-4 hour under high velocity agitation, be placed in stainless steel cauldron, in 110 DEG C of hydrothermal treatment consists 6h after sealing, suction filtration, washing, dry at 80 DEG C, grind for subsequent use;

(2) polypropene staple is put into butyl titanate and flood 2-5 hour, ovendry power is broken to 200-300 order, adds beta-alumina, sesbania powder and suitable quantity of water ultrasonic wave and dries for dispersion grinding 3-5 hour;

(3) by step (1), the mixing of (2) material, add other residual components and stir 30-50 minute, microwave drying grinding discharging in 3 hours at leaving standstill 1-5 hour, 160-180 DEG C.

The present invention has following beneficial effect: the present invention is raw materials used cheap and easy to get, stable performance, can be mass-produced, adopt aqueous potassium hydrogen sulfate to uniform load after the acidification of vermiculite surface on silica, form the covalent structure of stable Mg-O-Si and Ca-O-Si, loading process does not destroy SiO ₂structure and generate compound specific area larger, add polypropene staple particles stick at alumina surface simultaneously, improve adsorptivity, acid enhancing, low temperature active is good, the composite solid-acid catalyst utilizing the present invention to obtain solves the common fault of common metal oxides solid acid catalyst easy in inactivation, add sour density, acid strength is promoted greatly, and catalytic effect is excellent simultaneously, reusable, environmental friendliness.

Detailed description of the invention

Described a kind of low temperature high activity composite solid-acid catalyst, it is characterized in that, be made up of the raw material of following weight portion: beta-alumina 52, vermiculite 5, antimony oxide 9, silica 23, polypropene staple 16, potassium acid sulfate 2, butyl titanate 11, sesbania powder 8, suitable quantity of water.

Preparation method comprises the following steps:

(1) potassium acid sulfate is added water to be stirred to dissolve completely, add vermiculite and soak 10-12 hour, grinding pulping, add silica and flood absorption 2-4 hour under high velocity agitation, be placed in stainless steel cauldron, in 110 DEG C of hydrothermal treatment consists 6h after sealing, suction filtration, washing, dry at 80 DEG C, grind for subsequent use;

(2) polypropene staple is put into butyl titanate and flood 2-5 hour, ovendry power is broken to 200-300 order, adds beta-alumina, sesbania powder and suitable quantity of water ultrasonic wave and dries for dispersion grinding 3-5 hour;

(3) by step (1), the mixing of (2) material, add other residual components and stir 30-50 minute, microwave drying grinding discharging in 3 hours at leaving standstill 1-5 hour, 160-180 DEG C.

Claims (2)

1. a low temperature high activity composite solid-acid catalyst, it is characterized in that, be made up of the raw material of following weight portion: beta-alumina 48-55, vermiculite 4-6, antimony oxide 6-9, silica 20-24, polypropene staple 14-17, potassium acid sulfate 2-4, butyl titanate 10-13, sesbania powder 8-14, suitable quantity of water.

2. the preparation method of a kind of low temperature high activity composite solid-acid catalyst according to claim 1, is characterized in that comprising the following steps:

(1) potassium acid sulfate is added water to be stirred to dissolve completely, add vermiculite and soak 10-12 hour, grinding pulping, add silica and flood absorption 2-4 hour under high velocity agitation, be placed in stainless steel cauldron, in 110 DEG C of hydrothermal treatment consists 6h after sealing, suction filtration, washing, dry at 80 DEG C, grind for subsequent use;

(2) polypropene staple is put into butyl titanate and flood 2-5 hour, ovendry power is broken to 200-300 order, adds beta-alumina, sesbania powder and suitable quantity of water ultrasonic wave and dries for dispersion grinding 3-5 hour;

(3) by step (1), the mixing of (2) material, add other residual components and stir 30-50 minute, microwave drying grinding discharging in 3 hours at leaving standstill 1-5 hour, 160-180 DEG C.