CN106334516A - Antichlor and preparation method thereof - Google Patents
Antichlor and preparation method thereof Download PDFInfo
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- CN106334516A CN106334516A CN201610891768.1A CN201610891768A CN106334516A CN 106334516 A CN106334516 A CN 106334516A CN 201610891768 A CN201610891768 A CN 201610891768A CN 106334516 A CN106334516 A CN 106334516A
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- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
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- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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- B01D2257/202—Single element halogens
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Abstract
The invention provides an antichlor which comprises an active component and further comprises a carrier. The mass ratio of the carrier to the active component in antichlor raw materials is 0.7-1.5. The antichlor further comprises a bonder, a peptizer and a forming addition agent and the like. The invention further provides a method for preparing the antichlor. The method comprises the steps of performing mixing, band extrusion and drying on the active component, the carrier and the forming addition agent and the like and further comprises the step of roasting to obtain the formed antichlor. The obtained antichlor is high in compressive strength and large in penetrating chlorosity, hydrogen chloride in mixed gas can be effectively removed, an adverse effect on an oil refining device is reduced, the antichlor can be prepared in a short time under low temperature conditions, so that energy consumption is reduced, and the production cost is reduced.
Description
Technical field
A kind of the invention belongs to gas purification technique field, in particular it relates to antichlor and preparation method thereof.
Background technology
Recently as the increase of oil extraction depth, the heavy of crude oil, in poor quality are on the rise.Crude oil and its distillate
In chloride content be also in continuous to raise trend, chlorine corrosion, ammonium salt blockage, ammonium chloride underdeposit corrosion and chlorine that chloride causes
The problems such as compound stress corrosion cracking, brings a lot of potential safety hazards to oil refining apparatus.Therefore, to chlorination in crude oil and its distillate
The removing research of thing becomes inexorable trend.
Chloride in crude oil is divided into butter and organic chloride two class.Butter mainly with nacl,
mgcl2And cacl2Presented in alkali and alkaline earth metal ions salt, organic chloride is then mainly presented in chlorohydrocarbon.
Butter effectively can be removed by electric desalting apparatus before crude oil processing, and most organic chloride still can
It is present in crude oil, this part organic chloride can be converted into hydrogen chloride under certain condition, and then to production equipment and pipeline
Have undesirable effect, be mainly manifested in following three aspects: 1) hydrogen chloride gas are in relatively low ambient temperature and with the presence of condensed water
When, low temperature hcl-h can be formed2s-h2O corrosive environment, thus corrode refining equipment.This corrosion is primarily present in atmospheric and vacuum distillation unit
Fore-running column overhead, normal pressure column overhead, decompression column overhead, the equipment such as Atmospheric vacuum condenser system and the pre- hydrogenation system of catalytic reforming
In.2) chloride ion has higher electron affinity and animal migration, so easily reacting with metal ion, causes the permanent of catalyst
Poisoning, and chlorine can migrate downward into process fluid, complete so the harm to catalyst is often bed, so can be to enterprise
Industry brings larger economic loss.3) hydrogen chloride easily reacts generation ammonium chloride, ammonium chloride meeting under lower temperature conditions with ammonia
Crystallize and be deposited in the relevant devices such as pipeline, heat exchanger entrance, cause pipeline blockage, the normal operation of impact device, reduce
The service life of equipment.Therefore, muriatic removing, for long-term, the safe and stable operation of oil refining apparatus, improves Petrochemical Enterprises
Economic benefit significant.
The Chinese invention patent application of Publication No. cn104492368a is in order to solve antichlor low intensity, usage cycles
The problem that short, HCl content has much room for improvement, discloses a kind of antichlor, by using ferrous sulfate, calcium powder, high sulfur capacity powder is used as has
Effect raw material, thus carrying out reaction first with the calcium hydroxide in ferrous sulfate and calcium powder to generate FeOOH and calcium sulfate, will
FeOOH that above-mentioned reaction produces and the high sulfur capacity powder with FeOOH as main component that is directly added into collectively as
Active component, and give full play to the synergism between two kinds of active components, effectively improve the chlorosity of described antichlor;Meanwhile, also
Using the calcium sulfate with cementation producing in above-mentioned course of reaction so that duct in antichlor structure, specific surface area,
Active center distribution is all optimised, and can effectively improve the mechanical strength of antichlor, and antichlor of the present invention has relatively
High chlorosity and mechanical strength, analytical data shows, the chlorosity up to more than 65% of described antichlor, and mechanical strength is up to 100n/
More than cm.
But above antichlor comprcssive strength is relatively low, and (12mpa and more than) uses it is impossible under elevated pressure conditions, therefore, needs to make
Standby go out can (12mpa and more than) uses under elevated pressure conditions antichlor, ensure the long period safe and stable operation of refinery device.
Content of the invention
In order to overcome above technical problem of the prior art, the present invention provides a kind of antichlor and preparation method thereof, should
The comprcssive strength of antichlor is improved.
In order to reach object above, the present invention employs the following technical solutions: a kind of antichlor, its raw material includes activearm
Point, also include carrier.Add carrier in active component, so that the comprcssive strength of antichlor is got a promotion.
Preferably, the mass ratio of carrier described in the raw material of described antichlor and active component is 0.7 ~ 1.5, carrier with
In the ratio here of active component is interval, well putting down of antichlor comprcssive strength and chlorosity (especially penetrating chlorosity) can be obtained
Weighing apparatus.
Preferably, the raw material of described antichlor also includes shaping assistant to any of the above-described scheme.
Preferably, described shaping assistant includes binding agent to any of the above-described scheme.
Any of the above-described scheme preferably, percent that described binding agent accounts for active component and carrier gross mass is 30 ~
70wt.%.
Preferably, described binding agent includes Alumina gel, polyvinyl alcohol or Kaolin to any of the above-described scheme.
Preferably, described shaping assistant includes peptizer to any of the above-described scheme.
Any of the above-described scheme preferably, percent that described peptizer accounts for active component and carrier gross mass is 3 ~
7wt.%.
Preferably, described peptizer includes nitric acid, hydrochloric acid or acetic acid to any of the above-described scheme.
Preferably, described shaping assistant includes extrusion aid to any of the above-described scheme.
Any of the above-described scheme preferably, percent that described extrusion aid accounts for active component and carrier gross mass is 1 ~
3wt.%.
Preferably, described extrusion aid includes sesbania powder and/or polybasic carboxylic acid to any of the above-described scheme.
Preferably, the raw material of described antichlor also includes distilled water to any of the above-described scheme.
Preferably, the addition of described distilled water is gouache ratio (volume of distilled water and activearm to any of the above-described scheme
Divide the ratio with carrier gross mass) 0.1 ~ 0.5ml/g.Gouache ratio all has a significant impact to extruded velocity and comprcssive strength;Pigment
Ratio is big, the good fluidity of dough, and antichlor is easily extruded;But when gouache ratio is excessive, antichlor not easy-formation.For of the present invention
Antichlor, control gouache ratio in the range of 0.1 ~ 0.5ml/g when, you can ensure that antichlor has enough comprcssive strength and outer
See shape.
Preferably, described active component includes one or more of cao, mgo, zno and cuo to any of the above-described scheme
Metal composite oxide.This several metal-oxide or wherein several compound metal-oxide cao and zno or cao and mgo
Deng so that when it is as active component, the comprcssive strength of antichlor is improved.
Preferably, described active component is prepared any of the above-described scheme by urea coprecipitation method.Urea precipitation method
Prepared metal-oxide as antichlor active component so that the duct of antichlor, specific surface area and active center distribution
All preferable, and the comprcssive strength of antichlor can be effectively improved.
Preferably, described carrier is boehmite powder to any of the above-described scheme.
Preferably, described antichlor includes the active component of 30 ~ 70wt.% to any of the above-described scheme.
Preferably, described antichlor specific surface area is 100 ~ 130m to any of the above-described scheme2/g.
Preferably, the aperture of described antichlor is 5 ~ 8nm to any of the above-described scheme.
Preferably, the pore volume of described antichlor is 0.10 ~ 0.30cm to any of the above-described scheme3/g.
Preferably, the comprcssive strength of described antichlor is higher than 150n/cm to any of the above-described scheme.
The antichlor that the present invention provides, is to add carrier in active component so that the comprcssive strength of antichlor is carried
Height, meanwhile, adds shaping assistant so that antichlor has larger specific surface area, and makes its chlorosity, especially penetrate chlorosity and obtain
To improving, can reach more than 65%.In addition, selecting boehmite powder to be carrier, boehmite powder is through roasting under the high temperature conditions
Burning can generate γ-al2o3, γ-al2o3Antichlor can be made to keep higher chlorosity and gas purification degree.The dechlorination that the present invention provides
Agent, its comprcssive strength can reach more than 150n/cm, and penetrate chlorosity and can be increased substantially, and even as high as more than 65%.
On the other hand, the present invention also provides the preparation method of more than one antichlors, including by active component, carrier, one-tenth
The raw materials such as type auxiliary agent carry out mixing, extrusion, drying, also include carrying out roasting, obtain the antichlor of molding.
Preferably, described sintering temperature is 500 ~ 600 DEG C to any of the above-described scheme.
Preferably, described roasting time is 3 ~ 6h to any of the above-described scheme.
Preferably, the temperature of described drying is 100-120 DEG C to any of the above-described scheme.
Preferably, the time of described drying is 2 ~ 5h to any of the above-described scheme.
Any of the above-described scheme preferably, prepares described active component by urea coprecipitation method.Urea coprecipitation legal system
The metal-oxide obtaining has the advantages that particle diameter is little, is uniformly dispersed, specific surface area is big and chemical composition is homogeneous, using urea precipitation
The metal-oxide that method is obtained as antichlor active component so that the duct of antichlor, specific surface area, active center distribution
All preferable, and the comprcssive strength of antichlor can be effectively improved.
Any of the above-described scheme preferably, described preparation method, according to enforcement order, specifically include following steps successively:
(1) active component is prepared by urea coprecipitation method;
(2) active component, carrier, shaping assistant mix homogeneously are weighed;
(3) add distilled water, kneading becomes paste, and carries out extrusion, form the antichlor base substrate of molding;
(4) the antichlor base substrate of molding is dried;
(5) roasting is carried out to the antichlor base substrate being dried, obtain molding antichlor.
Antichlor preparation method in the present invention, prepares active component using urea coprecipitation method so that active component has
Have the advantages that particle diameter is little, be uniformly dispersed, specific surface area is big and chemical composition is homogeneous.Therefore, it is obtained using urea coprecipitation method
Metal-oxide as antichlor active component so that the duct of antichlor, specific surface area, active center distribution are all preferable,
And the comprcssive strength of antichlor can be effectively improved.
Antichlor preparation method of the present invention is by first by a certain amount of active component and shaping assistant and carrier
It is sufficiently mixed, is then kneaded into paste, then through extrusion, drying, roasting, the antichlor being so obtained is had higher resisting
Compressive Strength and the larger hydrogen chloride penetrating chlorosity, can effectively removing in mixed gas, reduce the harmful effect to oil refining apparatus.
Antichlor preparation method of the present invention, limits baking temperature as 100 ~ 120 DEG C, and drying time is 2 ~ 5h, roasting
Burn temperature and be 500 ~ 600 DEG C, roasting time is 3 ~ 6h.It is thereby achieved that under relatively low temperature conditionss and in the shorter time
Can be prepared by antichlor, so advantageously reduce energy expenditure, reduce production cost.
Specific embodiment
Content of the invention for a better understanding of the present invention, is further elaborated with reference to specific embodiment.
Agents useful for same of the present invention, such as nitrate, carbamide, nitric acid, hydrochloric acid, acetic acid etc., all can chemically Reagent Company buy.
Embodiment 1
A kind of antichlor, its preparing raw material includes: active component, carrier and shaping assistant.
In the present embodiment, described active component is the metal composite oxide of cao and mgo, and carrier is boehmite powder,
And carrier is 1.0 with the mass ratio of active component.Shaping assistant, according to the percent meter accounting for active component and carrier gross mass,
Binding agent for 50wt.%, the peptizer of 4wt.%, the extrusion aid of 1.5wt.%.
Raw material also includes the distilled water that gouache ratio is 0.2ml/g.
In the present embodiment, described binding agent is Alumina gel, is mainly used in strengthening the caking property of antichlor, to improve its resistance to compression
Intensity.Described peptizer is nitric acid, is on the one hand because that nitric acid can improve the pore structure of antichlor, on the other hand can improve dechlorination
The comprcssive strength of agent.Described extrusion aid is sesbania powder, and the addition of extrusion aid can make the smooth molding of antichlor.
The preparation method of this antichlor is as follows:
(1) the metal composite oxide active component of cao and mgo is prepared first with urea coprecipitation method: with carbamide as precipitant,
Itself and nitrate (calcium nitrate: magnesium nitrate=2:1, mol ratio) are placed in same conical flask and are made into mixed solution, then this is mixed
Close solution and be placed in water-bath and react and crystallization under the conditions of 80 ~ 100 DEG C, finally by this reactant mixture sucking filtration, filter cake distills
Water washing is to neutral, the prepared metal composite oxide active component of roasting after drying.Prepare activearm using urea coprecipitation method
Point, be primarily due to urea coprecipitation method be obtained metal composite oxide particle diameter little, be uniformly dispersed, specific surface area big and chemical
Uniform component.Therefore, the duct of antichlor, specific surface area, work can be made using the antichlor active component that urea precipitation method is obtained
Property central distribution is all preferable, and can effectively improve the comprcssive strength of antichlor.
(2) weigh the active component of certain mass, by carrier: active component=1.0(mass ratio) add boehmite
Powder, then crowded with helping of the 50% of carrier gross mass binding agent Alumina gel, 4% peptizer nitric acid and 1.5% by accounting for active component
Agent sesbania powder is mixed homogeneously with above-mentioned carrier and active component;
(3) gouache ratio pressing 0.2ml/g adds distilled water, and is kneaded into paste;
(4) use double screw banded extruder extruded moulding, obtain the antichlor of molding;
(5) antichlor of molding is dried;
(6) dried antichlor is carried out roasting, finally give the antichlor of molding.
In the present embodiment, drying is 5h to be dried under the conditions of 100 DEG C, and described roasting is roasting 6h under the conditions of 500 DEG C.
In the present embodiment, in the molding antichlor finally giving, cao is 40wt.%, and mgo is 20wt.%, and remaining is carrier
Content with shaping assistant.
In the present embodiment, the antichlor specific surface area of final molding is 120.973m2▪g-1, pore volume is 0.224cm3▪g-1,
Average pore size is 7.420nm.
The antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm, being passed through hcl content is
The nitrogen of 0.698mg/l, adsorption temp is set as 40 DEG C, is 2097h in hcl gas volume air speed-1Under conditions of evaluate de-
Chlorine agent penetrate chlorosity, draw the relation curve of hydrogen chloride content and time in exit gas, penetrate when the content of hcl reaches
The chlorosity that penetrates being calculated this antichlor during point (the 10% of hcl input concentration) is 17.12wt.%.
Measure the comprcssive strength of antichlor by chemical industry standard hg/t2782-2011, using global instrument plant of Jiangyan City
The kc-2 digital display granule strength instrument producing, takes the molding antichlor that 10 length are 5mm, measures the pressure resistance of every antichlor
Degree, result takes its arithmetic mean of instantaneous value, and result of calculation shows, the comprcssive strength of the molding antichlor finally giving in the present embodiment is
163n/cm.
Embodiment 2
A kind of antichlor, as different from Example 1, in the present embodiment, during preparation active component, calcium nitrate is rubbed with magnesium nitrate
Your ratio is 4:1, and carrier is 1.1 with the mass ratio of active component.
In the present embodiment, in the molding antichlor finally giving, the content of cao is 45wt.%, and the content of mgo is
15wt.%, remaining is carrier and shaping assistant.
In the present embodiment, the specific surface area of the molding antichlor finally giving is 116.3181m2▪g-1, pore volume is
0.192cm3▪g-1, average pore size is 6.605nm.
The antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm, being passed through hcl content is
The nitrogen of 0.698mg/l, adsorption temp is set as 40 DEG C, is 2097h in hcl gas volume air speed-1Under conditions of evaluate de-
The dechlorination of chlorine agent, draws the relation curve of hydrogen chloride content and time in exit gas, when the content of hcl reaches breakthrough point
The chlorosity that penetrates calculating this antichlor when (the 10% of hcl input concentration) is 26.53wt.%.
Measure the comprcssive strength of antichlor by chemical industry standard hg/t2782-2011, using global instrument plant of Jiangyan City
The kc-2 digital display granule strength instrument producing, takes the molding antichlor that 10 length are 5mm, measures the pressure resistance of every antichlor
Degree, result takes its arithmetic mean of instantaneous value, and result of calculation shows, the comprcssive strength of the molding antichlor finally giving in the present embodiment is
158n/cm.
Embodiment 3
A kind of antichlor, as different from Example 1, in the present embodiment, active component is single cao.Carrier and activearm
The mass ratio dividing is 0.9.
The preparation method of the antichlor in the present embodiment, on the basis of the preparation method of embodiment 1, nitrate is adjusted to
Individually calcium nitrate.
In the present embodiment, in the molding antichlor finally giving, the content of cao is 60wt.%, and remaining is carrier and molding
Auxiliary agent.
In the present embodiment, the specific surface area of the molding antichlor finally giving is 107.522m2▪g-1, pore volume is
0.150cm3▪g-1, average pore size is 5.579nm.
The antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm, being passed through hcl content is
The nitrogen of 0.698mg/l, adsorption temp is set as 40 DEG C, is 2097h in hcl gas volume air speed-1Under conditions of evaluate de-
The dechlorination of chlorine agent, draws the relation curve of hydrogen chloride content and time in exit gas, when the content of hcl reaches breakthrough point
The chlorosity that penetrates calculating this antichlor when (the 10% of hcl input concentration) is 46.93wt.%.
Measure the comprcssive strength of antichlor by chemical industry standard hg/t2782-2011, using global instrument plant of Jiangyan City
The kc-2 digital display granule strength instrument producing, takes the molding antichlor that 10 length are 5mm, measures the pressure resistance of every antichlor
Degree, result takes its arithmetic mean of instantaneous value, and result of calculation shows, the comprcssive strength of the molding antichlor finally giving in the present embodiment is
152n/cm.
Embodiment 4.1
As different from Example 3, the antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm,
It is passed through the nitrogen that hcl content is 0.698mg/l, adsorption temp is set as 40 DEG C, be 3355h in hcl gas volume air speed-1's
Under the conditions of the dechlorination of antichlor is evaluated, evaluation result shows that the chlorosity that penetrates of this antichlor is 32.91wt.%.
Embodiment 4.2
As different from Example 3, the antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm,
It is passed through the nitrogen that hcl content is 0.698mg/l, adsorption temp is set as 40 DEG C, be 4193h in hcl gas volume air speed-1's
Under the conditions of the dechlorination of antichlor is evaluated, evaluation result shows that the chlorosity that penetrates of this antichlor is 29.49wt.%.
Embodiment 4.3
As different from Example 3, the antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm,
It is passed through the nitrogen that hcl content is 1.496mg/l, adsorption temp is set as 40 DEG C, be 2097h in hcl gas volume air speed-1's
Under the conditions of the dechlorination of antichlor is evaluated, evaluation result is shown to be 52.49wt.%.
Embodiment 4.4
As different from Example 3, the antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm,
It is passed through the nitrogen that hcl content is 3.128mg/l, adsorption temp is set as 40 DEG C, be 2097h in hcl gas volume air speed-1's
Under the conditions of the dechlorination of antichlor is evaluated, evaluation result shows that the chlorosity that penetrates of this antichlor is 66.67wt.%.
This group embodiment is passed through to change operating condition, has investigated the gas volume air speed of containing hydrogen chloride and the gas of containing hydrogen chloride
Bulk concentration penetrates the impact of chlorosity to antichlor.
Embodiment 5.1
A kind of antichlor, its preparing raw material includes: active component, carrier and shaping assistant.
In the present embodiment, described active component is the metal composite oxide of cao and mgo.Carrier is boehmite powder,
And carrier is 0.9 with the mass ratio of active component.Shaping assistant, according to the percent meter accounting for active component and carrier gross mass,
The extrusion aid of the binding agent for 30wt.%, the peptizer of 3wt.% and 1.0wt.%.
Raw material also includes the distilled water that gouache ratio is 0.1ml/g.
In the present embodiment, described binding agent is Alumina gel, and described peptizer is nitric acid, and described extrusion aid is sesbania powder.
The preparation method of this antichlor is as follows:
(1) active component cao and mgo are prepared first with urea coprecipitation method: with carbamide as precipitant, by itself and nitrate
(calcium nitrate: magnesium nitrate=2:1, mol ratio) is configured to mixed solution, then this mixed solution is placed in water-bath at 80 ~ 100 DEG C
Under the conditions of reaction and crystallization, finally by this reactant mixture sucking filtration, filter cake is washed with distilled water to neutrality, after drying roasting be obtained
Metal composite oxide active component.
(2) weigh the active component of certain mass, by carrier: active component=0.9(mass ratio) add boehmite
Powder, then will account for the extrusion aid of the binding agent Alumina gel that active component is with carrier gross mass 30%, 3% peptizer nitric acid and 1.0%
Sesbania powder is mixed homogeneously with above-mentioned carrier and active component;
(3) gouache ratio pressing 0.1ml/g adds distilled water, and is kneaded into paste;
(4) use double screw banded extruder extruded moulding, obtain the antichlor of molding;
(5) antichlor of molding is dried;
(6) dried antichlor is carried out roasting, finally give the antichlor of molding.
In the present embodiment, drying is 3h to be dried under the conditions of 110 DEG C, and described roasting is roasting 4h under the conditions of 550 DEG C.
In the present embodiment, in the molding antichlor finally giving, cao is 40wt.%, and mgo is 20wt.%, and remaining is carrier
With shaping assistant.
In the present embodiment, the specific surface area of the antichlor of final molding is 120.973m2▪g-1, pore volume is 0.224cm3▪g-1, average pore size is 7.420nm.
The antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm, being passed through hcl content is
The nitrogen of 0.698mg/l, adsorption temp is set as 40 DEG C, is 2097h in hcl gas volume air speed-1Under conditions of evaluate de-
The dechlorination of chlorine agent, draws the relation curve of hydrogen chloride content and time in exit gas, when the content of hcl reaches breakthrough point
The chlorosity that penetrates calculating this antichlor when (the 10% of hcl input concentration) penetrates chlorosity for 41.89wt.%.
Measure the comprcssive strength of antichlor by chemical industry standard hg/t2782-2011, using global instrument plant of Jiangyan City
The kc-2 digital display granule strength instrument producing, takes the molding antichlor that 10 length are 5mm, measures the pressure resistance of every antichlor
Degree, result takes its arithmetic mean of instantaneous value, and result of calculation shows, the comprcssive strength of the antichlor of the molding finally giving in the present embodiment
For 153n/cm.
Embodiment 5.2
A kind of antichlor, its preparing raw material includes: active component, carrier and shaping assistant.
In the present embodiment, described active component is the metal composite oxide of cao and mgo, and carrier is boehmite powder,
And carrier is 1.2 with the mass ratio of active component.Shaping assistant, according to the percent meter accounting for active component and carrier gross mass,
Binding agent for 60wt.%, the peptizer of 5wt.%, the extrusion aid of 2wt.%.
Raw material also includes the distilled water that gouache ratio is 0.3ml/g.
In the present embodiment, described binding agent is Alumina gel, and described peptizer is nitric acid, and described extrusion aid is sesbania powder.
The preparation method of this antichlor is as follows:
(1) prepare the metal composite oxide active component of cao and mgo first with urea coprecipitation method: with carbamide for precipitation
Agent, itself and nitrate (calcium nitrate: magnesium nitrate=2:1, mol ratio) is configured to mixed solution, is then placed in this mixed solution
React and crystallization under the conditions of 80 ~ 100 DEG C in water-bath, finally by this reactant mixture sucking filtration, during filter cake is washed with distilled water to
Property, roasting after drying is obtained metal composite oxide active component.
(2) weigh the active component of certain mass, by carrier: active component=1.2(mass ratio) add boehmite
Powder, then will account for the extrusion aid of the 60% binding agent Alumina gel that active component is with carrier gross mass, 5% peptizer nitric acid and 2%
Sesbania powder is mixed homogeneously with above-mentioned carrier and active component;
(3) gouache ratio pressing 0.3ml/g adds distilled water, and is kneaded into paste;
(4) use double screw banded extruder extruded moulding, obtain the antichlor of molding;
(5) antichlor of molding is dried;
(6) dried antichlor is carried out roasting, finally give the antichlor of molding.
In the present embodiment, drying is 2h to be dried under the conditions of 120 DEG C, and described roasting is roasting 3h under the conditions of 600 DEG C.
In the present embodiment, in the molding antichlor finally giving, cao is 40wt.%, and mgo is 19wt.%, and remaining is carrier
With shaping assistant.
In the present embodiment, the antichlor specific surface area of final molding is 120.973m2▪g-1, pore volume is 0.224cm3▪g-1,
Average pore size is 7.420nm.
The antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm, being passed through hcl content is
The nitrogen of 0.698mg/l, adsorption temp is set as 40 DEG C, is 2097h in hcl gas volume air speed-1Under conditions of evaluate de-
The dechlorination of chlorine agent, draws the relation curve of hydrogen chloride content and time in exit gas, when the content of hcl reaches breakthrough point
The chlorosity that penetrates calculating this antichlor when (the 10% of hcl input concentration) is 18.26wt.%.
Measure the comprcssive strength of antichlor by chemical industry standard hg/t2782-2011, using global instrument plant of Jiangyan City
The kc-2 digital display granule strength instrument producing, takes the molding antichlor that 10 length are 5mm, measures the pressure resistance of every antichlor
Degree, result takes its arithmetic mean of instantaneous value, and result of calculation shows, the comprcssive strength of the molding antichlor finally giving in the present embodiment is
160n/cm.
Embodiment 5.3
A kind of antichlor, its preparing raw material includes: active component, carrier and shaping assistant.
In the present embodiment, described active component is the metal composite oxide of cao and mao.Carrier is boehmite powder,
And carrier is 1.4 with the mass ratio of active component.Shaping assistant, according to the percent meter accounting for active component and carrier gross mass,
Binding agent for 70wt.%, the peptizer of 6wt.%, the extrusion aid of 2.5wt.%.
Raw material also includes the distilled water that gouache ratio is 0.4ml/g.
In the present embodiment, described binding agent is Alumina gel, and described peptizer is nitric acid, and described extrusion aid is sesbania powder.
The preparation method of this antichlor is as follows:
(1) prepare the metal composite oxide active component of cao and mgo first with urea coprecipitation method: with carbamide for precipitation
Agent, itself and nitrate (calcium nitrate: magnesium nitrate=3:1, mol ratio) is configured to mixed solution, is then placed in this mixed solution
React and crystallization under the conditions of 80 ~ 100 DEG C in water-bath, finally by this reactant mixture sucking filtration, during filter cake is washed with distilled water to
Property, roasting after drying is obtained metal composite oxide active component.
(2) weigh the active component of certain mass, by carrier: active component=1.4(mass ratio) add boehmite
Powder, then will account for the extrusion aid of the binding agent Alumina gel that active component is with carrier gross mass 70%, 6% peptizer nitric acid and 2.5%
Fill out cyanines powder to mix homogeneously with above-mentioned carrier and active component;
(3) gouache ratio pressing 0.4ml/g adds distilled water, and is kneaded into paste;
(4) use double screw banded extruder extruded moulding, obtain the antichlor of molding;
(5) antichlor of molding is dried;
(6) dried antichlor is carried out roasting, finally give the antichlor of molding.
In the present embodiment, drying is 5h to be dried under the conditions of 110 DEG C, and described roasting is roasting 6h under the conditions of 550 DEG C.
In the present embodiment, in the molding antichlor finally giving, cao is 38wt.%, and mgo is 18wt.%, and remaining is carrier
With shaping assistant.
In the present embodiment, the antichlor specific surface area of final molding is 120.973m2▪g-1, pore volume is 0.224cm3▪g-1,
Average pore size is 7.420nm.
The antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm, being passed through hcl content is
The nitrogen of 0.698mg/l, adsorption temp is set as 40 DEG C, is 2097h in hcl gas volume air speed-1Under conditions of evaluate de-
The dechlorination of chlorine agent, draws the relation curve of hydrogen chloride content and time in exit gas, when the content of hcl reaches breakthrough point
The chlorosity that penetrates calculating this antichlor when (the 10% of hcl input concentration) is 17.09wt.%.
Measure the comprcssive strength of antichlor by chemical industry standard hg/t2782-2011, using global instrument plant of Jiangyan City
The kc-2 digital display granule strength instrument producing, takes the molding antichlor that 10 length are 5mm, measures the pressure resistance of every antichlor
Degree, result takes its arithmetic mean of instantaneous value, and result of calculation shows, the comprcssive strength of the molding antichlor finally giving in the present embodiment is
164n/cm.
Embodiment 5.4
A kind of antichlor, its preparing raw material includes: active component, carrier and shaping assistant.
In the present embodiment, described active component is the metal composite oxide of cao and mao, and carrier is boehmite powder,
And carrier is 1.5 with the mass ratio of active component.Shaping assistant, according to the percent meter accounting for active component and carrier gross mass,
Binding agent for 40wt.%, the peptizer of 7wt.%, the extrusion aid of 3wt.%.
Raw material also includes the distilled water that gouache ratio is 0.5ml/g.
In the present embodiment, described binding agent is Alumina gel, and described peptizer is nitric acid, and described extrusion aid is sesbania powder.
The preparation method of this antichlor is as follows:
(1) prepare the metal composite oxide active component of cao and mgo first with urea coprecipitation method: with carbamide for precipitation
Agent, itself and nitrate (calcium nitrate: magnesium nitrate=2:1, mol ratio) is configured to mixed solution, is then placed in this mixed solution
React and crystallization under the conditions of 80 ~ 100 DEG C in water-bath, finally by this reactant mixture sucking filtration, during filter cake is washed with distilled water to
Property, roasting after drying is obtained metal composite oxide active component.
(2) weigh the active component of certain mass, by carrier: active component=1.5(mass ratio) add boehmite
Powder, then will account for the extrusion aid field of the binding agent Alumina gel that active component is with carrier gross mass 40%, 7% peptizer nitric acid and 3%
Cyanines powder is mixed homogeneously with above-mentioned carrier and active component;
(3) gouache ratio pressing 0.5ml/g adds distilled water, and is kneaded into paste;
(4) use double screw banded extruder extruded moulding, obtain the antichlor of molding;
(5) antichlor of molding is dried;
(6) dried antichlor is carried out roasting, finally give the antichlor of molding.
In the present embodiment, drying is 2h to be dried under the conditions of 120 DEG C, and described roasting is roasting 3h under the conditions of 600 DEG C.
In the present embodiment, in the molding antichlor finally giving, cao is 38wt.%, and mgo is 17wt.%, and remaining is carrier
With shaping assistant.
In the present embodiment, the specific surface area of the antichlor of final molding is 120.973m2▪g-1, pore volume is 0.224cm3▪g-1, average pore size is 7.420nm.
The antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm, being passed through hcl content is
The nitrogen of 0.698mg/l, adsorption temp is set as 40 DEG C, is 2097h in hcl gas volume air speed-1Under conditions of evaluate de-
The dechlorination of chlorine agent, draws the relation curve of hydrogen chloride content and time in exit gas, when the content of hcl reaches breakthrough point
The chlorosity that penetrates calculating this antichlor when (the 10% of hcl input concentration) is 16.99wt.%.
Measure the comprcssive strength of antichlor by chemical industry standard hg/t2782-2011, using global instrument plant of Jiangyan City
The kc-2 digital display granule strength instrument producing, takes the molding antichlor that 10 length are 5mm, measures the pressure resistance of every antichlor
Degree, result takes its arithmetic mean of instantaneous value, and result of calculation shows, the comprcssive strength of the antichlor of the molding finally giving in the present embodiment
For 165n/cm.
Embodiment 5.5
A kind of antichlor, as different from Example 3, carrier is 0.7 with the mass ratio of active component.
In the present embodiment, in the molding antichlor finally giving, cao is 65wt.%, and remaining is carrier and shaping assistant.
In the present embodiment, the specific surface area of the antichlor of final molding is 107.526m2▪g-1, pore volume is 0.148cm3▪g-1, average pore size is 5.583nm.
The antichlor that particle diameter is 0.5 ~ 1.0mm is taken to load in the absorption fixed bed that internal diameter is 1.0cm, being passed through hcl content is
The nitrogen of 0.698mg/l, adsorption temp is set as 40 DEG C, is 2097h in hcl gas volume air speed-1Under conditions of evaluate de-
The dechlorination of chlorine agent, draws the relation curve of hydrogen chloride content and time in exit gas, when the content of hcl reaches breakthrough point
The chlorosity that penetrates calculating this antichlor when (the 10% of hcl input concentration) is 47.38wt.%.
Measure the comprcssive strength of antichlor by chemical industry standard hg/t2782-2011, using global instrument plant of Jiangyan City
The kc-2 digital display granule strength instrument producing, takes the molding antichlor that 10 length are 5mm, measures the pressure resistance of every antichlor
Degree, result takes its arithmetic mean of instantaneous value, and result of calculation shows, the comprcssive strength of the antichlor of the molding finally giving in the present embodiment
For 157n/cm.
Embodiment 6.1
A kind of antichlor, as different from Example 3, active component is mgo.
In the present embodiment, nitrate is adjusted to magnesium nitrate hexahydrate by the preparation method of antichlor accordingly.
Embodiment 6.2
A kind of antichlor, as different from Example 3, active component is cuo.
In the present embodiment, nitrate is adjusted to Gerhardite by the preparation method of antichlor accordingly.
Embodiment 6.3
A kind of antichlor, as different from Example 3, active component is zno.
In the present embodiment, nitrate is adjusted to zinc nitrate hexahydrate by the preparation method of antichlor accordingly.
Embodiment 6.4
A kind of antichlor, as different from Example 2, active component is the metal composite oxide of zno and cuo.
Nitrate is adjusted to zinc nitrate hexahydrate and three hydration nitre by the preparation method of antichlor accordingly in the present embodiment
Sour copper.
Embodiment 6.5
A kind of antichlor, as different from Example 2, active component is the metal composite oxide of mgo and cuo.
Nitrate is adjusted to magnesium nitrate hexahydrate and three hydration nitre by the preparation method of antichlor accordingly in the present embodiment
Sour copper.
Embodiment 6.6
A kind of antichlor, as different from Example 2, active component is the metal composite oxide of mgo and zno.
Nitrate is adjusted to magnesium nitrate hexahydrate and six hydration nitre by the preparation method of antichlor accordingly in the present embodiment
Sour zinc.
Embodiment 6.7
A kind of antichlor, as different from Example 2, active component is the metal composite oxide of cao and cuo.
Nitrate is adjusted to calcium nitrate tetrahydrate and three hydration nitre by the preparation method of antichlor accordingly in the present embodiment
Sour copper.
Embodiment 6.8
A kind of antichlor, as different from Example 2, active component is the metal composite oxide of cao and zno.
Nitrate is adjusted to calcium nitrate tetrahydrate and six hydration nitre by the preparation method of antichlor accordingly in the present embodiment
Sour zinc.
Embodiment 6.9
A kind of antichlor, as different from Example 1, active component is the metal composite oxide of cao, mgo and zno.
Nitrate is adjusted to calcium nitrate tetrahydrate, six hydration nitre by the preparation method of antichlor accordingly in the present embodiment
Sour magnesium and zinc nitrate hexahydrate, and mol ratio is 2:2:1.
Embodiment 6.10
A kind of antichlor, as different from Example 1, active component is the metal composite oxide of cao, mgo and zno.
Nitrate is adjusted to calcium nitrate tetrahydrate, six hydration nitre by the preparation method of antichlor accordingly in the present embodiment
Sour magnesium and zinc nitrate hexahydrate, and mol ratio is 3:1:1.
Embodiment 6.11
A kind of antichlor, as different from Example 1, active component is the metal composite oxide of cao, mgo and cuo.
Nitrate is adjusted to calcium nitrate tetrahydrate, six hydration nitre by the preparation method of antichlor accordingly in the present embodiment
Sour magnesium and Gerhardite, and mol ratio is 3:1:1.
Embodiment 6.12
A kind of antichlor, as different from Example 1, active component is the metal composite oxide of zno, mgo and cuo.
Nitrate is adjusted to zinc nitrate hexahydrate, six hydration nitre by the preparation method of antichlor accordingly in the present embodiment
Sour magnesium and Gerhardite, and mol ratio is 3:1:1.
Embodiment 7.1
A kind of antichlor, as different from Example 1, binding agent is polyvinyl alcohol.Preparation method is adjusted correspondingly.
Embodiment 7.2
A kind of antichlor, as different from Example 1, binding agent is Kaolin.Preparation method is adjusted correspondingly.
Embodiment 8.1
A kind of antichlor, as different from Example 1, peptizer is hydrochloric acid.Preparation method is adjusted correspondingly.
Embodiment 8.2
A kind of antichlor, as different from Example 1, peptizer is acetic acid.Preparation method is adjusted correspondingly.
Embodiment 9.1
A kind of antichlor, as different from Example 1, extrusion aid is oxalic acid.Preparation method is adjusted correspondingly.
Embodiment 9.2
A kind of antichlor, as different from Example 1, extrusion aid is citric acid.Preparation method is adjusted correspondingly.
Embodiment 9.3
A kind of antichlor, as different from Example 1, extrusion aid is tartaric acid.Preparation method is adjusted correspondingly.Embodiment
9.4
A kind of antichlor, as different from Example 1, extrusion aid is sesbania powder and oxalic acid.Preparation method is adjusted correspondingly.
Embodiment 9.5
A kind of antichlor, as different from Example 1, extrusion aid is sesbania powder and citric acid.Preparation method is adjusted accordingly
Whole.
Embodiment 9.6
A kind of antichlor, as different from Example 1, extrusion aid is sesbania powder and tartaric acid.Preparation method is adjusted accordingly
Whole.
Comparative example 1
Scheme disclosed in Chinese invention patent application according to Publication No. cn104492368a, obtains the antichlor compareing,
Penetrate chlorosity evaluation methodology according to the antichlor in embodiment 1 to be evaluated, the chlorosity that penetrates obtaining is only 12.38wt.%.Press
The antichlor comprcssive strength obtaining according to the measuring method of comprcssive strength in embodiment 1 is 99.98n/cm.
Comparative example 2
According to scheme disclosed in embodiment in the Chinese invention patent application of Publication No. cn105617853a 4, obtain comparison de-
Chlorine agent, penetrates chlorosity evaluation methodology according to the antichlor in the embodiment of the present invention 4.4 and is evaluated, and the comparison antichlor obtaining is worn
Chlorosity is 58.73wt.% thoroughly.The comparison antichlor comprcssive strength that measuring method according to comprcssive strength in embodiment 1 obtains is
108.34n/cm.
Comparative example 3
A kind of antichlor, as different from Example 1, the metal composite oxide of cao and mgo, using commercially available cao and mgo
(Chemical Reagent Co., Ltd., Sinopharm Group), other steps are identical.Antichlor penetrate chlorosity and intensity test also with reality
Apply the comparison antichlor that example 1 is identical, obtains, penetrating chlorosity is 10.02wt.%, and comprcssive strength is 138n/cm.
Comparative example 4
A kind of antichlor, as different from Example 3, as the cao of single-activity component, using commercially available cao.Antichlor
The chlorosity that penetrates penetrating the comparison antichlor that chlorosity is identical with embodiment 4.4 with intensity test, obtains is 21.74wt.%,
Comprcssive strength is 118n/cm.
Comparative example 5
A kind of antichlor, as different from Example 3, carrier is 1.6:1 with the mass ratio of active component.Antichlor penetrate chlorine
Hold identical with embodiment 4.4 with intensity test, the chlorosity that penetrates of the comparison antichlor obtaining is 30.17wt.%, pressure resistance
Spend for 167n/cm.
Comparative example 6
A kind of antichlor, as different from Example 3, carrier is 2.0:1 with the mass ratio of active component.Antichlor penetrate chlorine
Hold identical with embodiment 4.4 with intensity test, the chlorosity that penetrates of the comparison antichlor obtaining is 19.97wt.%, pressure resistance
Spend for 189n/cm.
Comparative example 7
A kind of antichlor, as different from Example 3, carrier is 0.4:1 with the mass ratio of active component.Antichlor penetrate chlorine
Hold identical with embodiment 4.4 with intensity test, the chlorosity that penetrates of the comparison antichlor obtaining is 57.21wt.%, pressure resistance
Spend for 141n/cm.
Comparative example 8
A kind of antichlor, as different from Example 3, carrier is 0.2:1 with the mass ratio of active component.Antichlor penetrate chlorine
Hold identical with embodiment 4.4 with intensity test, the chlorosity that penetrates of the comparison antichlor obtaining is 63.74wt.%, pressure resistance
Spend for 126n/cm.
Thus, it is possible to find out, the antichlor that the present invention provides, comprcssive strength is improved, and meanwhile, also improves low temperature bar
The dechlorination efficiency penetrating chlorosity, greatly increasing antichlor of antichlor under part, has ensured that refinery device is efficient, stable, has pacified
Entirely run.
It should be noted that various embodiments above, only in order to technical scheme to be described, is not intended to limit;Although
With reference to foregoing embodiments, the present invention has been described in detail, those of ordinary skill in the art it should be understood that: its
Still the technical scheme described in foregoing embodiments can be modified, or to wherein some or all of technical characteristic
Carry out equivalent;And these modifications or replacement, do not make the essence of appropriate technical solution depart from various embodiments of the present invention skill
The scope of art scheme.
Claims (10)
1. a kind of antichlor, its raw material include active component it is characterised in that: also include carrier.
2. antichlor as claimed in claim 1 it is characterised in that: carrier and active component described in the raw material of described antichlor
Mass ratio be 0.7 ~ 1.5.
3. antichlor as claimed in claim 2 it is characterised in that: the raw material of described antichlor also includes shaping assistant.
4. antichlor as claimed in claim 3 it is characterised in that: described shaping assistant includes binding agent.
5. antichlor as claimed in claim 4 it is characterised in that: described binding agent account for active component with carry gross mass percentage
Number is 30 ~ 70wt.%.
6. antichlor as claimed in claim 5 it is characterised in that: described binding agent includes Alumina gel, polyvinyl alcohol or kaolinite
Soil.
7. antichlor as claimed in claim 6 it is characterised in that: described shaping assistant includes peptizer.
8. antichlor as claimed in claim 7 it is characterised in that: described peptizer accounts for the hundred of active component and carrier gross mass
Fraction is 3 ~ 7wt.%.
9. antichlor as claimed in claim 8 it is characterised in that: described peptizer includes nitric acid, hydrochloric acid or acetic acid.
10. a kind of preparation method of antichlor as claimed in any one of claims 1-9 wherein, including by active component, carrier, one-tenth
The raw materials such as type auxiliary agent carry out mixing, extrusion, drying it is characterised in that: also include carrying out roasting, obtain antichlor.
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CN115487838A (en) * | 2022-08-05 | 2022-12-20 | 中国石油化工股份有限公司 | Hydrodechlorination catalyst, catalyst system and hydrofining process method of high-chlorine-content waste plastic cracking oil |
CN115350576A (en) * | 2022-09-20 | 2022-11-18 | 大唐环境产业集团股份有限公司 | Supported magnesium oxide dechlorinating agent and preparation method and application thereof |
CN115888804A (en) * | 2022-11-10 | 2023-04-04 | 山东嘉盛博纳环保科技有限公司 | Dechlorinating agent and preparation method thereof |
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