CN103771735B - White lime process polyolefin catalyst titanium-containing waste residues is utilized to prepare the method for cement - Google Patents

White lime process polyolefin catalyst titanium-containing waste residues is utilized to prepare the method for cement Download PDF

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CN103771735B
CN103771735B CN201210401191.3A CN201210401191A CN103771735B CN 103771735 B CN103771735 B CN 103771735B CN 201210401191 A CN201210401191 A CN 201210401191A CN 103771735 B CN103771735 B CN 103771735B
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cement
containing waste
titanium
waste residues
white lime
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CN103771735A (en
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邢毅
李昕阳
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

Abstract

White lime process polyolefin catalyst titanium-containing waste residues is utilized to prepare the method for cement.The invention provides a kind of recycling processing method for polyolefin catalyst titanium-containing waste residues, utilize white lime powder titanium-containing waste residues directly to carry out mixing and reacting, then fully react with water again, a kind of slurries of final generation, and leave standstill for some time after fixing.Finally cured article is burned in cement rotary kiln, remove noxious pollutant, utilize effective constituent wherein simultaneously, use as cement clinker.The object of the invention is to solve amount of hydrolysis water in prior art large, react violent, uppity problem, and due in sodium hydroxide and a large amount of titanium oxide of producing of the hydrolyzed solution of titanium-containing waste residues and organic pollutant, reduce subsequent wastewater treatment difficulty.

Description

White lime process polyolefin catalyst titanium-containing waste residues is utilized to prepare the method for cement
Technical field:
The invention belongs to the recycling treatment field of industrial residue, relating to a kind of recycling processing method of polyolefin catalyst titanium-containing waste residues, relating more specifically to a kind of recycling processing method of the waste residue such as titanium tetrachloride and high boiling material to producing in polyolefin catalyst preparation process.
Background technology
Ziegler-Natta catalyst is a kind of organo-metallic catalyst be most widely used in polyolefin industry.The preparation of this catalyzer is mixed mutually by the solid carrier of titanium tetrachloride and magnesium-containing compound or catalyst precursor to reach right times, finally obtains highly active Ziegler-Natta catalyst component.And the salvage stores such as the titanium tetrachloride be not loaded into and high boiling material is by hydrocarbon solvent washing removing, be catalyzer mother liquor.Wherein, high boiling material mainly comprises high boiling substance such as (halo) titan-alkoxide, lipid etc.
For the treatment process of catalyzer mother liquor, the titanium tetrachloride in current domestic main employing distillating method recovery catalyzer mother liquor and hydrocarbon solvent.Wherein, the lower hydrocarbon solvent of boiling point comparatively easily in a distillation column with other Component seperation, but to be only just discharged in the retort of flow process end due to the high boiling material in catalyzer mother liquor, easily tower bottom to be divided, reboiler and tower internals cause fouling and obstruction.And along with the raising of the titanium tetrachloride rate of recovery, the high boiling material proportions such as (halo) titan-alkoxide also can increase, and cause salvage stores viscosity higher, poor fluidity, once overstand easily causes the coking of still wall at high operating temperatures thereupon.Therefore, in order to the normal operation of assurance device, the rate of recovery of titanium tetrachloride is unsuitable excessive, and distillation temperature can not be too high, and the residence time of catalyzer mother liquor should be not long.
For the waste residue that retort is discharged, treatment process conventional is at present entered hydrolysis kettle hydrolysis, the hydrochloric acid then utilizing in sodium hydroxide and formed.But utilize such treatment process, hydrolysis reaction is gentle not, the more difficult control of whole operation.Meanwhile, the water yield that the reaction that is hydrolyzed consumes is huge, and the waste water quality produced is complicated, and containing a large amount of titanium oxide and organic pollutant, processing cost is high.The particularly existence of a large amount of chlorion in waste water, adds subsequent wastewater treatment difficulty.
Summary of the invention
In order to solve exist in prior art utilize hydrolysis reaction process titanium-containing waste residues water consumption large, react violent, wayward, and produce the problem of a large amount of titanium oxide and organic pollutant with the hydrolyzed solution of titanium-containing waste residues in use sodium hydroxide, reduce subsequent wastewater treatment difficulty, the invention provides a kind of white lime process polyolefin catalyst titanium-containing waste residues that utilizes to prepare the method for cement.
The invention provides a kind of white lime process polyolefin catalyst titanium-containing waste residues that utilizes to prepare the method for cement, comprise following steps:
1) in reactor, white lime powder and titanium-containing waste residues is added, mix and react, wherein, temperature of reaction is 50 ~ 150 DEG C, reaction times is 2 ~ 8 hours, in described white lime powder, calcium hydroxide content is in butt more than 80%, and moisture is less than 5%, and the dosage of described titanium-containing waste residues and the mass ratio of white lime powder are 1:0.2 ~ 1:10; Be preferably 1:1 ~ 1:3.
2) in reactor, add water, with accelerated reaction process, and make the more abundant of material reaction, the final one that obtains is containing TiO 2, CaCl 2in the slurries of material.The mass ratio of water and the interior total material of reactor is 1:0.5 ~ 1:5; Be preferably 1:0.8 ~ 1:2.Reaction times is 0.5 ~ 2 hour.
3) the described slurries obtained after reaction are placed 6 ~ 72 hours after fixing, described slurries change cured article into.
4) cured article obtained is pulverized, send in cement rotary kiln and burn, and supplement cement slurry, be prepared into cement clinker.Wherein, the mass ratio of cement slurry and cured article is 5:1 ~ 100:1.
Described titanium-containing waste residues comprises the titanium tetrachloride that content is 5wt% ~ 80wt%, content is (halo) titan-alkoxide of 2wt% ~ 80wt%, and content is the by product of 0wt% ~ 20wt%, wherein said (halo) titan-alkoxide is titan-alkoxide and/or halogenated alkoxy titanium.
Described (halo) titan-alkoxide can use general formula TiX m(OR) nexpression, wherein X is halogen, be preferably chlorine, R is the low alkyl group with 1 ~ 10 carbon atom, preferred ethyl, n-propyl, sec.-propyl, normal-butyl, isobutyl-, the tertiary butyl, n-pentyl, isopentyl tert-pentyl, wherein m=0 ~ 3, n=1 ~ 4,2≤m+n≤4.
Described by product comprises aliphatics (two) ester and/or aromatic series (two) ester and their derivative, particularly, mainly comprise diisobutyl phthalate, 2, the two benzoic ethers of 4 pentanediols etc., described aliphatics (two) ester is aliphatic diester and/or aliphatic ester, and described aromatic series (two) ester is aromatic diester and/or aromatic ester.
Reactor in the present invention is preferably mixing machine or kneader, because containing solid slag in the pollutent of process, easily cake mass is formed in simultaneous reactions process, so in order to react time mixing more fully and after reaction blowing smooth and easy, the reactor types of intensive shear, mixing effect can be produced solid-state or semi-solid state material, general stirring reactor should not be selected.More preferably spiral mixer is used.
Described temperature of reaction by controlling with the reactor of water jacket and the speed that adds of control titanium-containing waste residues, can control between 50 ~ 150 DEG C to make temperature of reaction.
Inorganic component in described cured article comprises CaCl 2nH 2o, TiO 2, Ca (OH) 2.
Described cement rotary kiln is the best type of furnace of burning Hazardous wastes, particularly combustible waste.The volume of cement rotary kiln is comparatively large, stable conditions, calcining temperature are high, and waste material can stop for a long time in kiln, and does not have secondary pollutant to discharge.In addition, cement rotary kiln also can utilize the combustibility of waste residue to it can be used as complementarity alternative fuel, reduces fuel source consumption.
Described cement clinker, in its component, content of titanium dioxide is less than 2wt%, and calcium chloride content is at 0.5wt% ~ 2wt%.Wherein, titanium dioxide, as the trace element in cement, has good mineralization, and as cement setting retarder, alternative dihydrate gypsum is to the effect of cement.Calcium chloride, as cement slurry, can play the effect of acceleration of hydration, have good remineralization efficacy to the silicate in cement and aluminate.
Described cement clinker can be used for solidifying disposal of wastes, then landfill, effectively can prevent the outflow of penetrating fluid.
To the regulation of chemical index, physical index, intensity and fineness if described cement clinker cement products meets technical requirements in standard GB/T 175-2007, construction cement can be directly used in and use.
In the present invention, calcium hydroxide directly can react with the titanium tetrachloride etc. in titanium-containing waste residues, and its thermal discharge then uses in sodium hydroxide and hydrochloric acid institute liberated heat much smaller than being first hydrolyzed through hydrolysis kettle, therefore, the reaction of calcium hydroxide and titanium-containing waste residues is more gentle, easily controls.Meanwhile, calcium hydroxide is also conventional curing/stabilizing material, and calcium hydroxide is also conventional curing/stabilizing material, the objectionable constituent in refuse can be adsorbed, absorbs, is wrapped up, and final formation has the cured article of some strength.
The invention has the beneficial effects as follows:
1) the present invention directly processes titanium-containing waste residues by white lime, and adds a certain amount of water with the process of accelerated reaction, experienced by multiple steps such as mixing, reaction, solidification altogether, finally realizes the minimizing to titanium-containing waste residues, harmlessness disposing.
2) adopt calcium hydroxide to replace the conventional sodium hydroxide used, release of heat is little, reacts gentleer, the use of calcium hydroxide not only effectively can remove the materials such as unmanageable titanium tetrachloride, and other noxious pollutants can be wrapped up, finally form cured article, be convenient to storage and transport.
3) change into the disposal options of titanium-containing waste residues directly mix with white lime by being hydrolyzed neutralization, then add water fully reaction, and its water consumption comparatively hydrolytic process greatly reduces.
4) reacted by white lime slurries, both added the degree of mixing of material, improve speed of response, also reduce the mixing resistance of reactor, reduce the use power of reactor; Meanwhile, white lime setting rate is slow, intensity is low, is convenient to reacted material to carry out shifting and transporting.
5) the final cured article formed decreases final treatment of wastes produced amount, is convenient to storage and transport.
6) by the mode that cement rotary kiln burns, be compared to land-fill method, transudate can be prevented the pollution of edatope.
7) using refuse as cement slurry, be prepared into cement clinker, realize the recycle of resource, cement products after preparation can be used for solidification treatment refuse, reducing the spilling of penetrating fluid, when meeting cement national standard, can directly use as construction cement.
By the present invention, not only reduce the expense of process polypropylene catalyst waste residue, and too increase income by preparation sale cement products, compare to the traditional treatment method to polypropylene catalyst waste residue, effectively saved cost.
Embodiment
Embodiment 1:
The present embodiment uses autohemagglutination third hydrocarbon catalyst titanium-containing waste residues that retort produces, wherein titanium tetrachloride content 50wt%, Chloroethoxy titanium content 40wt%, the by-products content 10wt% such as diisobutyl phthalate.The white lime used in the present embodiment, calcium hydroxide content (in butt) 98wt%, moisture is lower than 1%.Reactor in the present embodiment selects the double-spiral conical mixer of 15L.
The experimental procedure of the present embodiment:
1) in mixing machine, 3kg white lime powder is added;
2) divided by the titanium-containing waste residues of 3kg several times to pass in above-mentioned mixing machine, mix and react with white lime powder, temperature of reaction controls at 90 DEG C ~ 100 DEG C, 5 hours reaction times.
3) in mixing machine, 3L water is added, 1.5 hours reaction times.Final acquisition one is containing TiO 2, CaCl 2in the slurries of material.
4) reaction rear slurry is placed 24 hours after fixing, reaction rear slurry changes cured article into.
5) cured article is pulverized, and send into burning in cement rotary kiln, and supplement cement slurry 880kg, be prepared into cement clinker.Wherein, in cement clinker, titanium dioxide accounts for 1.2wt%, and calcium chloride accounts for 1.6wt%.
Cement clinker product after preparation meets technical requirements in standard GB/T 175-2007 and, to the regulation of chemical index, physical index, intensity and fineness, can be directly used in construction cement and use.
Embodiment 2:
The present embodiment uses autohemagglutination third hydrocarbon catalyst titanium-containing waste residues that retort produces, wherein titanium tetrachloride content 5wt%, Chloroethoxy titanium content 80wt%, the by-products content 15wt% such as diisobutyl phthalate.The white lime used in the present embodiment, calcium hydroxide content (in butt) 90wt%, moisture is lower than 2%.Reactor in the present embodiment selects the double-spiral conical mixer of 15L.
The experimental procedure of the present embodiment:
1) in mixing machine, 4kg white lime powder is added;
2) pass in above-mentioned mixing machine by the titanium-containing waste residues of 0.4kg, mix and react with white lime slurries, temperature of reaction controls at 50 DEG C ~ 80 DEG C, 2 hours reaction times.
3) in mixing machine, 0.9L water is added, 2 hours reaction times.Final acquisition one is containing TiO 2, CaCl 2in the slurries of material.
4) reaction rear slurry is placed 6 hours after fixing, reaction rear slurry changes cured article into.
5) cured article is pulverized, and send into burning in cement rotary kiln, and supplement cement slurry, be prepared into cement clinker 53kg.Wherein, in cement clinker, titanium dioxide accounts for 0.6wt%, and calcium chloride accounts for 0.9wt%.
Cement clinker product after preparation processes refuse by curing, effectively can prevent the spilling of penetrating fluid in refuse.
Embodiment 3:
The present embodiment uses autohemagglutination third hydrocarbon catalyst titanium-containing waste residues that retort produces, wherein titanium tetrachloride content 80wt%, Chloroethoxy titanium content 2wt%, the by-products content 18wt% such as diisobutyl phthalate.The white lime used in the present embodiment, calcium hydroxide content (in butt) 80wt%, moisture is lower than 5%.Reactor in the present embodiment selects the kneader of 25L.
The experimental procedure of the present embodiment:
1) in kneader, 5kg white lime powder is added;
2) pass in above-mentioned kneader by the titanium-containing waste residues of 3kg, mix and react with white lime slurries, temperature of reaction controls at 120 DEG C ~ 150 DEG C, 8 hours reaction times.
3) in kneader, 16L water is added, 0.5 hour reaction times.Final acquisition one is containing TiO 2, CaCl 2in the slurries of material.
4) reaction rear slurry is placed 72 hours after fixing, reaction rear slurry changes cured article into.
5) cured article is pulverized, and send into burning in cement rotary kiln, and supplement cement slurry, be prepared into cement clinker 120kg.Wherein, in cement clinker, titanium dioxide accounts for 0.5wt%, and calcium chloride accounts for 2wt%.
Cement clinker product after preparation processes refuse by curing, effectively can prevent the spilling of penetrating fluid in refuse.
Embodiment 4:
The present embodiment uses autohemagglutination third hydrocarbon catalyst titanium-containing waste residues that retort produces, wherein titanium tetrachloride content 67wt%, chloro n-butoxy titanium content 33wt%, the by-products content 0wt% such as diisobutyl phthalate.The white lime used in the present embodiment, calcium hydroxide content (in butt) 85wt%, moisture is lower than 3%.Reactor in the present embodiment selects the kneader of 25L.
The experimental procedure of the present embodiment:
1) in kneader, 6kg white lime powder is added;
2) pass in above-mentioned kneader by the titanium-containing waste residues of 2kg, mix and react with white lime slurries, temperature of reaction controls at 100 DEG C ~ 110 DEG C, 6 hours reaction times.
3) in kneader, 8L water is added, 2 hours reaction times.Final acquisition one is containing TiO 2, CaCl 2in the slurries of material.
4) reaction rear slurry is placed 24 hours after fixing, reaction rear slurry changes cured article into.
5) cured article is pulverized, and send into burning in cement rotary kiln, and supplement cement slurry, be prepared into cement clinker 800kg.Wherein, in cement clinker, titanium dioxide accounts for 0.2wt%, and calcium chloride accounts for 0.6wt%.
Cement clinker product after preparation processes refuse by curing, effectively can prevent the spilling of penetrating fluid in refuse.
Embodiment 5:
The present embodiment uses autohemagglutination third hydrocarbon catalyst titanium-containing waste residues that retort produces, wherein titanium tetrachloride content 29wt%, Chloroethoxy titanium content 51wt%, the by-products content 20wt% such as diisobutyl phthalate.The white lime used in the present embodiment, calcium hydroxide content (in butt) 90wt%, moisture is lower than 2%.Reactor in the present embodiment selects the mixing machine of 15L.
The experimental procedure of the present embodiment:
1) in mixing machine, 1kg white lime powder is added;
2) pass in above-mentioned mixing machine by the titanium-containing waste residues of 5kg, mix and react with white lime slurries, temperature of reaction controls at 75 DEG C ~ 95 DEG C, 4 hours reaction times.
3) in mixing machine, 2L water is added, 1 hour reaction times.Final acquisition one is containing TiO 2, CaCl 2in the slurries of material.
4) reaction rear slurry is placed 48 hours after fixing, reaction rear slurry changes cured article into.
5) cured article is pulverized, and send into burning in cement rotary kiln, and supplement cement slurry, be prepared into cement clinker 650kg.Wherein, in cement clinker, titanium dioxide accounts for 0.4wt%, and calcium chloride accounts for 0.3wt%.
Cement clinker product after preparation meets technical requirements in standard GB/T 175-2007 and, to the regulation of chemical index, physical index, intensity and fineness, can be directly used in construction cement and use.
Embodiment 6:
The present embodiment uses autohemagglutination third hydrocarbon catalyst titanium-containing waste residues that retort produces, wherein titanium tetrachloride content 82wt%, Chloroethoxy titanium content 15wt%, the by-products content 3wt% such as diisobutyl phthalate.The white lime used in the present embodiment, calcium hydroxide content (in butt) 90wt%, moisture is lower than 2%.Reactor in the present embodiment selects the double-spiral conical mixer of 15L.
The experimental procedure of the present embodiment:
1) in mixing machine, 4kg white lime powder is added;
2) pass in above-mentioned mixing machine by the titanium-containing waste residues of 2kg, mix and react with white lime slurries, temperature of reaction controls at 80 DEG C ~ 100 DEG C, 6 hours reaction times.
3) in mixing machine, 7.5L water is added, 2 hours reaction times.Final acquisition one is containing TiO 2, CaCl 2in the slurries of material.
4) reaction rear slurry is placed 60 hours after fixing, reaction rear slurry changes cured article into.
5) cured article is pulverized, and send into burning in cement rotary kiln, and supplement cement slurry, be prepared into cement clinker 280kg.Wherein, in cement clinker, titanium dioxide accounts for 0.9wt%, and calcium chloride accounts for 1.3wt%.
Cement clinker product after preparation processes refuse by curing, effectively can prevent the spilling of penetrating fluid in refuse.

Claims (10)

1. utilize white lime process polyolefin catalyst titanium-containing waste residues to prepare a method for cement, comprise following steps:
1) in reactor, white lime powder and titanium-containing waste residues is added, mix and react, wherein, temperature of reaction is 50 ~ 150 DEG C, reaction times is 2 ~ 8 hours, in described white lime powder, calcium hydroxide content is in butt more than 80%, and moisture is less than 5wt%, and the dosage of described titanium-containing waste residues and the mass ratio of described white lime powder are 1:0.2 ~ 1:10;
2) in reactor, add water, react after 0.5 ~ 2 hour, obtain containing TiO 2, CaCl 2slurries, wherein, in water and reactor, the mass ratio of total material is 1:0.5 ~ 1:5;
3), after the described slurries obtained after reaction being placed 6 ~ 72 hours, cured article is cured as;
4) pulverized by the cured article obtained, send in cement rotary kiln and burn, and supplement cement slurry, be prepared into cement clinker, wherein, the mass ratio of described cement slurry and cured article is 5:1 ~ 100:1.
2. utilize white lime process polyolefin catalyst titanium-containing waste residues to prepare the method for cement as claimed in claim 1, it is characterized in that, described titanium-containing waste residues comprises the titanium tetrachloride that content is 5wt% ~ 80wt%, content is (halo) titan-alkoxide of 2wt% ~ 80wt%, and content is the by product of 0wt% ~ 20wt%.
3. utilize white lime process polyolefin catalyst titanium-containing waste residues to prepare the method for cement as claimed in claim 2, it is characterized in that, described (halo) titan-alkoxide can use general formula TiX m(OR) nexpression, wherein X is halogen, and R is the low alkyl group with 1 ~ 10 carbon atom, m=0 ~ 3, n=1 ~ 4,2≤m+n≤4.
4. utilize white lime process polyolefin catalyst titanium-containing waste residues to prepare the method for cement as claimed in claim 2, it is characterized in that, described by product comprises aliphatic ester and/or aromatic ester and their derivative.
5. utilize white lime process polyolefin catalyst titanium-containing waste residues to prepare the method for cement as claimed in claim 1, it is characterized in that, step 1) described in the dosage of titanium-containing waste residues and the mass ratio of described white lime powder be 1:1 ~ 1:3.
6. utilize white lime process polyolefin catalyst titanium-containing waste residues to prepare the method for cement as claimed in claim 1, it is characterized in that, step 2) in water and reactor always the mass ratio of material be 1:0.8 ~ 1:1.2.
7. utilize white lime process polyolefin catalyst titanium-containing waste residues to prepare the method for cement as claimed in claim 1, it is characterized in that, described reactor is mixing machine or kneader.
8. utilize white lime process polyolefin catalyst titanium-containing waste residues to prepare the method for cement as claimed in claim 7, it is characterized in that, described mixing machine is mixing screw.
9. utilize white lime process polyolefin catalyst titanium-containing waste residues to prepare the method for cement as claimed in claim 1, it is characterized in that, described reactor is the reactor with water jacket.
10. the white lime process polyolefin catalyst titanium-containing waste residues that utilizes as described in any one of claim 1 ~ 9 prepares the method for cement, it is characterized in that, obtained cement clinker can be used for solidified waste and landfill or use as construction cement.
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CN104148359B (en) * 2014-07-07 2016-04-06 巨化集团技术中心 A kind of method of carbide slag process waste fluorination catalyst
CN106745308A (en) * 2016-12-14 2017-05-31 攀枝花钢企欣宇化工有限公司 The recovery and treatment method of titanium tetrachloride dust-slag collection
CN107739081B (en) * 2017-10-30 2020-04-14 四川宏达股份有限公司 Environment-friendly treatment process for titanium tetrachloride residual feed liquid
CN112851155B (en) * 2021-03-08 2022-07-08 葛洲坝石门特种水泥有限公司 Method for producing white cement clinker by using chemical waste residues and improving whiteness and strength of white cement clinker
JP6979145B1 (en) * 2021-04-30 2021-12-08 東邦チタニウム株式会社 Titanium component recovery method and titanium oxide manufacturing method

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