A kind of activating and regenerating method for the sand that decolourizes

文档序号:1747742 发布日期:2019-11-29 浏览:26次 中文

阅读说明:本技术 一种脱色砂的活化再生方法 (A kind of activating and regenerating method for the sand that decolourizes ) 是由 王俊武 廖晓宁 冯超 于 2019-09-24 设计创作,主要内容包括:本发明公开了一种脱色砂的活化再生方法,包括以下步骤:取废脱色砂和有机溶剂,将废脱色砂和有机溶剂按照体积比为1:2-7混合搅拌,得混合物;将所得混合物于30-55℃条件下超声处理5-15min,过滤,得脱色砂滤饼,然后将其干燥脱剂,得干燥脱色砂;向干燥脱色砂中加1-1.5倍干燥脱色砂重量的水将其分散,再依次向其中加入氧化剂和催化剂,于65-75℃条件下搅拌反应15-45min,过滤,得固体脱色砂,将固体脱色砂干燥,制得。该再生方法可有效解决现有的方法存在的洗脱过程水量消耗大,洗脱后脱色砂循环利用次数少的问题。(The invention discloses a kind of activating and regenerating methods of sand that decolourizes, comprising the following steps: takes useless decoloration sand and organic solvent, according to volume ratio is that 1:2-7 is mixed by useless decoloration sand and organic solvent, obtains mixture;Gained mixture is ultrasonically treated 5-15min under the conditions of 30-55 DEG C, is filtered, must decolourize sand filtration cake, then be dried de- agent, must dry decoloration sand;Into dry decoloration sand plus the water of 1-1.5 times of dry decoloration sand weight is dispersed, then oxidant and catalyst are successively added thereto, and 15-45min is stirred to react under the conditions of 65-75 DEG C, is filtered, solid decoloration sand is obtained, and solid decoloration sand is dry, is made.The regeneration method can effectively solve that elution process water content consumption existing for existing method is big, and elution rear decoloring sand recycles the few problem of number.)

1. a kind of activating and regenerating method for the sand that decolourizes, which comprises the following steps:

(1) useless decoloration sand and organic solvent are taken, useless decoloration sand and organic solvent are mixed according to the ratio that volume ratio is 1:2-7 and stirred It mixes, obtains mixture;

(2) mixture obtained by step (1) is ultrasonically treated under the conditions of 30-55 DEG C 5-15min, filtered, must decolourize sand filtration cake, so After be dried de- agent, must dry decoloration sand;

(3) add the water of 1-1.5 times of dry decoloration sand weight into dry decoloration sand obtained by step (2), then be successively added thereto Then oxidant and catalyst are stirred to react 15-45min under the conditions of 65-75 DEG C, filtering, obtain solid decoloration sand, solid is taken off Smalt is dry, is made;Wherein the additional amount of oxidant is equal with the dry decoloration quality of sand, and the additional amount of catalyst accounts for oxidant The 0.1-0.3% of quality.

2. as described in claim 1 decoloration sand activating and regenerating method, which is characterized in that in step (1) give up decoloration sand with have The volume ratio of solvent is 1:3.

3. the activating and regenerating method of decoloration sand as described in claim 1, which is characterized in that organic solvent described in step (1) For at least two in petroleum ether, ethyl alcohol, methyl acetate, ethyl acetate, acetone, hexamethylene, n-hexane and normal heptane.

4. the activating and regenerating method of decoloration sand as claimed in claim 3, which is characterized in that organic solvent described in step (1) It is mixed for the ratio that petroleum ether, methyl acetate and normal heptane are 1:6-9:9-15 by volume.

5. the activating and regenerating method of decoloration sand as described in claim 1, which is characterized in that the supersonic frequency in step (2) is 75-85KHz, ultrasonic power 65-75W.

6. the activating and regenerating method of decoloration sand as described in claim 1, which is characterized in that oxidant described in step (3) is Hydrogen peroxide, volumetric concentration 10%-30%.

7. the activating and regenerating method of decoloration sand as described in claim 1, which is characterized in that catalyst described in step (3) is Fe2+、Cu2+Or Mn2+

8. the activating and regenerating method of decoloration sand as claimed in claim 6, which is characterized in that the catalyst in step (3) is Fe2 +

9. the activating and regenerating method of decoloration sand as claimed in claim 7 or 8, which is characterized in that step will joined in (3) The dry decoloration sand of water, catalyst and oxidant is stirred to react 35min under 70 DEG C, UV irradiation condition, wherein UV irradiation power For 4-7W.

10. the activating and regenerating method of decoloration sand as described in claim 1, which is characterized in that the useless decoloration sand is to lubrication Substance after oil decolorization.

Technical field

The present invention relates to decoloration sand technical fields, and in particular to a kind of activating and regenerating method for the sand that decolourizes.

Background technique

In waste lubricating oil subtractive process, in order to which except the middle unstable compound that deoils, common processing method has plus hydrogen essence System, solvent extraction, adsorption bleaching.Wherein, hydrofinishing products obtained therefrom property is the most stable, and product quality is preferable, but there are skills The problems such as art threshold is excessively high, and equipment investment is high, and operation risk is big, at present hydrogenation technique external hydrogenation technique technology more at It is ripe, using most;Solvent extraction common are furfural extraction, phenol refining, NMP extracting, and effect is preferably NMP purification, but Solvent extraction cost is larger, and operational process key point corrosion phenomenon is serious, and recycling design acid value gradually rises, and will affect purification Oil quality;The active carclazyte of the most common adsorbent of adsorption refining, silica gel, atlapulgite is because of large specific surface area, adsorption effect It is good and the most commonly used, but there is recycling difficulty in spent bleaching clay, and therefore solidification disposal of waste problem at high cost generally passes through burning at present Or the method for landfill handles it, causes the great wasting of resources and environmental hazard.

Decoloration sand has the characteristics that performance is high, thermal stability is good, chemical property is stable, high mechanical strength, and has abundant Pore structure and biggish specific surface area, can replace completely atlapulgite for waste lubricating oil distillate post-refining, take off The advantages of smalt has decolorizing efficiency high, and wear rate is small, and regeneration rear decoloring works well, reuse number is up to 20 times, oil Product high income, and the decoloration sand after failure can be used for making waterglass, white carbon black, silica gel product etc., make solid waste Regeneration is obtained, is turned harm into good, is turned waste into wealth.

The regeneration method of useless silica decoloration sand usually under the high temperature conditions carries out decoloration sand using deionized water at present Then cleaning removes the oil body under elution, repeated washing is multiple, and the decoloration sand after cleaning is dry, is made.But this kind is again Generation method cannot completely elute the oil body adhered in the sand that decolourizes, and the decolorizing effect of the decoloration sand after leading to regeneration is poor, At most it is merely able to circulation decoloration 8 times;Moreover, a large amount of water can be expended when eluting under the high temperature conditions using deionized water, simultaneously In water body can also residual harmful substance, after discharge into water, certain pollution can be caused to environment.

Summary of the invention

For above-mentioned deficiency in the prior art, the present invention provides a kind of activating and regenerating method of sand that decolourizes, the regeneration It is big that method can effectively solve elution process water content consumption existing for existing method, and it is few that elution rear decoloring sand recycles number Problem.

To achieve the above object, the technical solution adopted by the present invention to solve the technical problems is:

A kind of activating and regenerating method for the sand that decolourizes, comprising the following steps:

(1) useless decoloration sand and organic solvent are taken, useless decoloration sand and organic solvent are mixed according to the ratio that volume ratio is 1:2-7 Stirring is closed, mixture is obtained;

(2) mixture obtained by step (1) is ultrasonically treated under the conditions of 30-55 DEG C 5-15min, filters, obtains decoloration sand filtration Then cake is dried de- agent, must dry decoloration sand;

(3) add the water of 1-1.5 times of dry decoloration sand weight into dry decoloration sand obtained by step (2), then successively thereto Oxidant and catalyst is added, 15-45min is then stirred to react under the conditions of 65-75 DEG C, filters, obtains solid decoloration sand, will consolidate Body decoloration sand is dry, is made;Wherein the additional amount of oxidant is equal with the dry decoloration quality of sand, and the additional amount of catalyst accounts for oxygen The 0.1-0.3% of agent quality.

Further, the volume ratio of useless decoloration sand and organic solvent is 1:3 in step (1).

Further, organic solvent described in step (1) is petroleum ether, ethyl alcohol, methyl acetate, ethyl acetate, acetone, ring At least two in hexane, n-hexane and normal heptane.

Further, it is 1:6- that organic solvent described in step (1) is petroleum ether, methyl acetate and normal heptane by volume The ratio of 9:9-15 is mixed.

Further, the supersonic frequency in step (2) is 75-85KHz, ultrasonic power 65-75W.

Further, oxidant described in step (3) is hydrogen peroxide, volumetric concentration 10%-30%.

Further, catalyst described in step (3) is Fe2+、Cu2+Or Mn2+

Further, the catalyst in step (3) is Fe2+

Further, the dry decoloration sand that joined water, catalyst and oxidant is irradiated in 70 DEG C, UV in step (3) Under the conditions of be stirred to react 35min, wherein UV irradiation power be 4-7W.

Further, the decoloration sand that gives up is to the substance after lubrication oil decolorization.

It takes and is had the beneficial effect that caused by above scheme

The method according to the invention carries out activating and regenerating to useless decoloration sand, overcomes present in existing washing regenerative process Water content consumption is big, regenerates the problem of deoiling effect difference, reduces the risk that regenerative process pollutes the environment, and is guaranteeing to decolourize Under the premise of refining basic oil quality, the decoloration sand after regeneration is recycled number and is up to 20 times.

Using organic solvent petroleum ether, methyl acetate and normal heptane as extractant in the present invention, wherein petroleum ether is to table Layer oil has dissolution diadochy well, and methyl acetate and normal heptane have very well the polar substances adsorbed in decoloration sand hole road Penetrate solvability, three's collective effect makes the lipid solubilization adsorbed in useless decoloration sand in organic solvent, can be improved useless Decolourize the discharge rate of grease in sand, and oxidant and catalyst, oxidant then, which will be added, into treated decoloration sand will take off What is adsorbed in smalt is not easy the substance fallen by organic solvent washing oxidation, and catalyst decomposes excessive oxidant, is keeping While oxidant higher utilization efficiency, the dosage of ferrous ion is reduced, and then reduces ferric iron and the attachment of decoloration sand is contaminated Color and to recycling decoloration sand decolorizing effect adverse effect, pass through the hole inside oxidant and catalyst depth purification and decoloration sand Road, the consumption so that organic matter for being not easy to be desorbed inside decoloration sand is degraded, so that decoloration sand restores the performance of adsorption bleaching.

Specific embodiment

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