CN105727903B - A kind of modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride - Google Patents
A kind of modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride Download PDFInfo
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- CN105727903B CN105727903B CN201610087741.7A CN201610087741A CN105727903B CN 105727903 B CN105727903 B CN 105727903B CN 201610087741 A CN201610087741 A CN 201610087741A CN 105727903 B CN105727903 B CN 105727903B
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Abstract
The invention discloses a kind of modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride, it is characterised in that diatomite is pre-processed；Diatomite is prepared into porous diatomite again；Then again by diatomite surface organic；Finally, then divide in heroic spirit, deionized water is added by following composition mass percent：24 ~ 34%, dimethyl diallyl ammonium chloride：42 ~ 52%, stirring and dissolving, add the porous diatomite that organises：18 ~ 28%, it is well mixed, azo-bis-iso-dimethyl：2 ~ 5%, each component sum is absolutely, in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 6 ~ 8, separation of solid and liquid after cooling, solid after separation is washed with deionized, untill being washed till filtrate in neutrality, filtering, dry, obtain the modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride.The adsorbent has very high adsorption capacity, excellent physical chemistry and mechanical performance to grease, and power of regeneration is strong, and often, not only cost was low but also green for Reusability.
Description
Technical field
The present invention relates to a kind of preparation method of adsorbent, belong to water-treatment technology field, the oil removing suitable for oil-polluted water
Purification, the modified porous diatomaceous preparation method of more particularly to a kind of dimethyl diallyl ammonium chloride and its in water process
In application.
Background technology
Increasing to the demand of oil with the industrialized rapid development in China, the use more next moon of oil product is extensive,
Generate and largely contain sewage.Oily waste water is mainly derived from oil recovery, oil refining, store oil, transport and the oil of petroleum industry
The processes such as Chemical Manufacture, after oil product enters water body, moisture film can be formed on top layer, prevent oxygen from dissolving in water body, so as to cause water body
Anoxic, biological death, cause serious environmental pollution.China promulgates at present《People's Republic of China's law of marine environmental protection》
Etc. rules and regulations, oily waste water highest allows concentration of emission to be 10 mg/L.So oily waste water is treated as oil instantly
The multiple fields urgent problem to be solved such as chemical industry and environmental protection.Absorption method is one kind in numerous handling process, in recent years
Carry out both at home and abroad research of many scholars to absorption method processing oily waste water to focus mostly in the adsorption efficiency of raising adsorbent, probe into suction
Attached dose method of modifying etc..Its absorption method has the features such as technique is simple, and adsorption rate is high, applied widely, and property is stable in dirt
It is used widely in water process.For the active charcoal of adsorbent of oily waste water absorption, expanded graphite, modified alta-mud, change
Property flyash, serpentine, attapulgite, zeolite etc..Gao Sainan etc. have studied the suction of oil extraction waste water biological treatment water outlet activated carbon
Adhesion test,（Environmental science and technologies are studied in the oil extraction waste water biological treatment water outlets such as Gao Sainan charcoal test,
2010-12,33(12): 56 – 65）；Wang Shuzhao etc. have studied absorption property of the expanded graphite to oily waste water,（Wang Shuzhao
Study on adsorption properties scientific and technical innovation Leader .2012 (22) Deng expanded graphites to oily waste water:7-8）；Shu Ming bravely waits research
The experiment of modified alta-mud processing emulsifying liquid waste water, Shu Ming bravely wait the experiment of modified alta-muds processing emulsifying liquid waste water to grind
Study carefully Chemical Engineers, 2012 (8): 34-38）；Deng Hui etc. have studied the application that flyash removes oily waste water,（Deng Hui etc. I
State removes the application study flyash of oily waste water, 2012 (3) using flyash: 10-14）.
Shortage of resources and environmental pollution have become two big subject matters of the world today, therefore, using natural resources, open
Send out feasible, green economy, environmentally friendly product and technology can strengthen China by as the inexorable trend of sustainable development
Tackle the strained handling ability of sudden serious contamination accident, to environmental protection, maintain the ecological balance, safeguard social safety with it is steady
Surely have a very important role.Diatom is a kind of single celled algae, individual very little, generally 1 μm to several millimeters.When this
After water plant death, remains can deposit in ocean in lake, form diatomite.Diatomite mineralogically belongs to opal knot
Structure, its chemical composition are mainly silica, contain a small amount of aluminum oxide, iron oxide, calcium oxide, magnesia, potassium oxide, oxidation
Sodium and organic matter.Diatomite is a kind of porous, density is small, specific surface area is big, excellent adsorption, the Optimality such as high temperature resistant, insulation
Matter, therefore it is widely used in the industrial circles such as chemical industry, oil, building materials, food.But the application field of some special absorption
It is higher to diatomaceous quality and performance requirement, though and China's diatomite ore aboundresources, quality be not universal high, permitted it
Many applications are restricted.Therefore, diatomaceous purification, modification are to improve the important means of diatomite application.The application
Chemical modification is carried out to porous diatomite using dimethyl diallyl ammonium chloride and prepares a kind of material of oil suction for sewage
In water process, diatomaceous new application is developed.
Dimethyl diallyl ammonium chloride, colourless transparent liquid, soluble in water, ethanol, there is excellent performance, extremely low thorn
Swash the quaternary surfactant of property, this product is a kind of bifunctional compound, containing alkyl functional group and allyl functionality, tool
There is excellent oil absorbency.The material being modified with dimethyl diallyl ammonium chloride has very strong lipophile, is to inhale well
Light wood material.
Through retrieval, have no using the modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride, and answered
Use absorption report oily in sewage disposal.
The content of the invention
An object of the present invention is to provide a kind of modified porous diatomaceous preparation side of dimethyl diallyl ammonium chloride
Method, another object is that the modified porous diatomite of the dimethyl diallyl ammonium chloride of preparation is applied at waste water as adsorbent
In reason.
The purpose of the present invention is achieved through the following technical solutions.
A kind of modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride, it is characterised in that this method has
Following processing step：
（1）Diatomaceous pretreatment：Sieve by diatomite with 120 mesh, it is 1g by solid-to-liquid ratio：4mL, by diatom
Soil is added to 1mol/L H2SO4In the aqueous solution, 30 min are boiled, after cooling, filtering, neutrality is washed with water to, dries, obtain pre-
Handle diatomite；
（2）Porous diatomite：In grinder, added by following composition mass percent：Pre-process diatomite：80~
85%, phenolic resin：5 ~ 10%, activated carbon：5 ~ 10%, calcium stearate：1 ~ 5%, each component sum is absolutely, opening grinds
Machine, 40 ~ 60min is ground with 500 turns/min rotating speed, 850 ~ 950 DEG C are placed in after taking-up, 3 ~ 4h is calcined, obtains porous diatomite；
（3）Organise porous diatomite：In the reactor, added by following composition mass percent：Absolute ethyl alcohol：46~
56%, VTES：16 ~ 26%, stirring and dissolving, add porous diatomite：22 ~ 32%, each component sum is hundred
/ hundred, temperature rises to 50 ~ 60 DEG C, and the h of back flow reaction 6 ~ 8, after cooling, separation of solid and liquid, the solid after separation is washed with deionized water
Wash, untill being washed till filtrate in neutrality, dry, obtain the porous diatomite that organises；
（4）The modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride：In the reactor, by following composition
Mass percent adds deionized water：24 ~ 34%, dimethyl diallyl ammonium chloride：42 ~ 52%, stirring and dissolving, add organic
Change porous diatomite：18 ~ 28%, it is well mixed, azo-bis-iso-dimethyl：2 ~ 5%, each component sum is a hundred per cent, in
65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 6 ~ 8, separation of solid and liquid after cooling, the solid after separation are washed with deionized, are washed till
Untill filtrate is in neutrality, filter, dry, obtain the modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride.
Step（3）Described in filtrate after separation of solid and liquid add the 3- r-chloropropyl trimethoxyl silicon of 5 ~ 8% mass percents again
After alkane, it can be continuing with.
It is a further object of the present invention to provide using the modified porous diatomite of the dimethyl diallyl ammonium chloride of preparation as
Adsorbent is applied to grease in waste water and handled, and grease includes in waste water：Crude oil, diesel oil, lubricating oil, machine oil, vegetable oil, gasoline.
Application method includes Static Adsorption and Dynamic Adsorption：The dimethyl diallyl ammonium chloride prepared is modified porous
Diatomite soaks 1 ~ 2h with deionized water, is adsorbed by static method；Adsorbed by dynamic method, adsorbent is loaded into adsorption column, containing grease
Waste water pass through by 5.0 mL/min of flow velocity.
Advantages of the present invention and effect are：
（1）The modified porous diatomite of dimethyl diallyl ammonium chloride that the present invention obtains has good physical chemistry steady
Qualitative and excellent mechanical strength, adsorption capacity is big, and maximum adsorption capacity 242mg/g, Reusability number is up to more than 10 times；
（2）The modified porous diatomite of dimethyl diallyl ammonium chloride that the present invention obtains is to various greases in water body（Such as
Crude oil, diesel oil, lubricating oil, machine oil, vegetable oil, gasoline etc.）There are preferably absorption and elution, adsorption efficiency is high, the speed of absorption
It hurry up, desorption performance is good, can be used in the range of wider soda acid；
（3）The condition for crossing range request of synthesis is easily controlled, and energy consumption is low, simple to operate, renewable resource utilization, is easy to industry
Metaplasia is produced.
Embodiment
Embodiment 1
（1）Diatomaceous pretreatment：Sieve by diatomite with 120 mesh, it is 1g by solid-to-liquid ratio：4mL, by diatom
Soil is added to 1mol/L H2SO4In the aqueous solution, 30 min are boiled, after cooling, filtering, neutrality is washed with water to, dries, obtain pre-
Handle diatomite；
（2）Porous diatomite：In grinder, it is separately added into：Pre-process diatomite：80g, phenolic resin：10g, activity
Charcoal：8g, calcium stearate：2g, grinder is opened, 50min is ground with 500 turns/min rotating speed, 900 DEG C are placed in after taking-up, calcining
3.5h, obtain porous diatomite；
（3）Organise porous diatomite：In the reactor, it is separately added into, absolute ethyl alcohol：63mL, vinyl triethoxyl
Silane：20g, stirring and dissolving, add porous diatomite：30g, temperature rise to 55 DEG C, back flow reaction 7h, after cooling, solid-liquid point
From the solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, dries, obtains the porous diatomite that organises；
（4）The modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride：In the reactor, it is separately added into,
Deionized water：30mL, dimethyl diallyl ammonium chloride：46g, stirring and dissolving, add the porous diatomite that organises：21g, mix
Close uniform, azo-bis-iso-dimethyl：3g, in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 7, separation of solid and liquid after cooling, divide
Solid from after is washed with deionized, and untill being washed till filtrate in neutrality, filters, dries, obtain dimethyl diallyl chlorination
The modified porous diatomaceous preparation method of ammonium.
Embodiment 2
（1）Diatomaceous pretreatment：Sieve by diatomite with 120 mesh, it is 1g by solid-to-liquid ratio：4mL, by diatom
Soil is added to 1mol/L H2SO4In the aqueous solution, 30 min are boiled, after cooling, filtering, neutrality is washed with water to, dries, obtain pre-
Handle diatomite；
（2）Porous diatomite：In grinder, it is separately added into：Pre-process diatomite：85g, phenolic resin：8g, activity
Charcoal：6g, calcium stearate：1g, grinder is opened, 60min is ground with 500 turns/min rotating speed, 950 DEG C are placed in after taking-up, calcining
3h, obtain porous diatomite；
（3）Organise porous diatomite：In the reactor, it is separately added into, absolute ethyl alcohol：70mL, vinyl triethoxyl
Silane：22g, stirring and dissolving, add porous diatomite：22g, temperature rise to 50 DEG C, back flow reaction 6h, after cooling, solid-liquid point
From the solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, dries, obtains the porous diatomite that organises；
（4）The modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride：In the reactor, it is separately added into,
Deionized water：34mL, dimethyl diallyl ammonium chloride：44g, stirring and dissolving, add the porous diatomite that organises：18g, mix
Close uniform, azo-bis-iso-dimethyl：4g, in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 6, separation of solid and liquid after cooling, divide
Solid from after is washed with deionized, and untill being washed till filtrate in neutrality, filters, dries, obtain dimethyl diallyl chlorination
The modified porous diatomaceous preparation method of ammonium.
Embodiment 3
（1）Diatomaceous pretreatment：Sieve by diatomite with 120 mesh, it is 1g by solid-to-liquid ratio：4mL, by diatom
Soil is added to 1mol/L H2SO4In the aqueous solution, 30 min are boiled, after cooling, filtering, neutrality is washed with water to, dries, obtain pre-
Handle diatomite；
（2）Porous diatomite：In grinder, it is separately added into：Pre-process diatomite：81g, phenolic resin：7g, activity
Charcoal：10g, calcium stearate：2g, grinder is opened, 40min is ground with 500 turns/min rotating speed, 850 DEG C are placed in after taking-up, calcining
4h, obtain porous diatomite；
（3）Organise porous diatomite：In the reactor, it is separately added into, absolute ethyl alcohol：58mL, vinyl triethoxyl
Silane：26g, stirring and dissolving, add porous diatomite：28g, temperature rise to 60 DEG C, back flow reaction 8h, after cooling, solid-liquid point
From the solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, dries, obtains the porous diatomite that organises；
（4）The modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride：In the reactor, it is separately added into,
Deionized water：24mL, dimethyl diallyl ammonium chloride：52g, stirring and dissolving, add the porous diatomite that organises：22g, mix
Close uniform, azo-bis-iso-dimethyl：2g, in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 8, separation of solid and liquid after cooling, divide
Solid from after is washed with deionized, and untill being washed till filtrate in neutrality, filters, dries, obtain dimethyl diallyl chlorination
The modified porous diatomaceous preparation method of ammonium.
Embodiment 4
（1）Diatomaceous pretreatment：Sieve by diatomite with 120 mesh, it is 1g by solid-to-liquid ratio：4mL, by diatom
Soil is added to 1mol/L H2SO4In the aqueous solution, 30 min are boiled, after cooling, filtering, neutrality is washed with water to, dries, obtain pre-
Handle diatomite；
（2）Porous diatomite：In grinder, it is separately added into：Pre-process diatomite：84g, phenolic resin：6g, activity
Charcoal：5g, calcium stearate：5g, grinder is opened, 45min is ground with 500 turns/min rotating speed, 900 DEG C are placed in after taking-up, calcining
3h, obtain porous diatomite；
（3）Organise porous diatomite：In the reactor, it is separately added into, absolute ethyl alcohol：60mL, vinyl triethoxyl
Silane：25g, stirring and dissolving, add porous diatomite：27g, temperature rise to 55 DEG C, back flow reaction 6h, after cooling, solid-liquid point
From the solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, dries, obtains the porous diatomite that organises；
（4）The modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride：In the reactor, it is separately added into,
Deionized water：28mL, dimethyl diallyl ammonium chloride：42g, stirring and dissolving, add the porous diatomite that organises：25g, mix
Close uniform, azo-bis-iso-dimethyl：5g, in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 6.5, separation of solid and liquid after cooling,
Solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, filters, dries, obtain dimethyl diallyl chlorine
Change the modified porous diatomaceous preparation method of ammonium.
Embodiment 5
（1）Diatomaceous pretreatment：Sieve by diatomite with 120 mesh, it is 1g by solid-to-liquid ratio：4mL, by diatom
Soil is added to 1mol/L H2SO4In the aqueous solution, 30 min are boiled, after cooling, filtering, neutrality is washed with water to, dries, obtain pre-
Handle diatomite；
（2）Porous diatomite：In grinder, it is separately added into：Pre-process diatomite：83g, phenolic resin：5g, activity
Charcoal：9g, calcium stearate：3g, grinder is opened, 50min is ground with 500 turns/min rotating speed, 900 DEG C are placed in after taking-up, calcining
4h, obtain porous diatomite；
（3）Organise porous diatomite：In the reactor, it is separately added into, absolute ethyl alcohol：65mL, vinyl triethoxyl
Silane：16g, stirring and dissolving, add porous diatomite：32g, temperature rise to 60 DEG C, back flow reaction 8h, after cooling, solid-liquid point
From the solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, dries, obtains the porous diatomite that organises；
（4）The modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride：In the reactor, it is separately added into,
Deionized water：26mL, dimethyl diallyl ammonium chloride：43g, stirring and dissolving, add the porous diatomite that organises：28g, mix
Close uniform, azo-bis-iso-dimethyl：3g, in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 7.5, separation of solid and liquid after cooling,
Solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, filters, dries, obtain dimethyl diallyl chlorine
Change the modified porous diatomaceous preparation method of ammonium.
Embodiment 6
Weigh the modified porous diatomite adsorbing material of 1.0g dimethyl diallyl ammonium chlorides and be placed in 250mL conical flask with cover
In, adding 100mL concentration is in 1000mg/L machine oil solution, using the pH value of acid or alkali regulation system as in the range of 4.0 ~ 10,
0.5 ~ 2 h of concussion absorption at room temperature, takes supernatant, concentration oily in solution is determined with infrared spectrum oil content analyzer, before absorption
Concentration difference oily in water afterwards, the modified porous diatomaceous adsorption capacity of dimethyl diallyl ammonium chloride is calculated, it, which is adsorbed, holds
Amount can reach 242mg/g, and pH value adsorbent in the range of 6.5 ~ 7.5 is maximum to the adsorption capacity of oil and stably, in room
Lower concussion absorption more than the 0.5h of temperature, absorption of the adsorbent to oil reach saturation.
Embodiment 7
Weigh the modified porous diatomite adsorbing material of 1.0g dimethyl diallyl ammonium chlorides and be placed in 250mL conical flask with cover
In, it is in 100mg/L solution containing machine oil to add 100mL concentration, using the pH value of acid or alkali regulation system as 7.0, is shaken at room temperature
1 h of absorption is swung, takes supernatant, oily concentration in solution is determined with infrared spectrum oil content analyzer, according to oily dense in water before and after absorption
Degree is poor, calculates clearance of the modified porous diatomite adsorbing material of dimethyl diallyl ammonium chloride to oil, reaches as high as
98.9%。
Claims (3)
1. a kind of modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride, it is characterised in that this method has
Following processing step：
(1) diatomaceous pretreatment：Sieve by diatomite with 120 mesh, it is 1g by solid-to-liquid ratio：4mL, diatomite is added
To 1mol/L H2SO4In the aqueous solution, 30min is boiled, after cooling, filtering, neutrality is washed with water to, dries, obtains pre-processing silicon
Diatomaceous earth；
(2) porous diatomite：In grinder, added by following composition mass percent：Pre-process diatomite：80~85%,
Phenolic resin：5~10%, activated carbon：5~10%, calcium stearate：1~5%, each component sum is absolutely, opening grinds
Machine, 40~60min is ground with 500 turns/min rotating speed, 850~950 DEG C are placed in after taking-up, 3~4h is calcined, obtains porous diatom
Soil；
(3) organise porous diatomite：In the reactor, added by following composition mass percent：Absolute ethyl alcohol：46~
56%, VTES：16~26%, stirring and dissolving, add porous diatomite：22~32%, each group divides it
50~60 DEG C, 6~8h of back flow reaction, after cooling are risen to for a hundred per cent, temperature, separation of solid and liquid, the solid after separation is spent
Ion water washing, untill being washed till filtrate in neutrality, dry, obtain the porous diatomite that organises；
(4) the modified porous diatomaceous preparation method of dimethyl diallyl ammonium chloride：In the reactor, by following composition quality
Percentage adds deionized water：24~34%, dimethyl diallyl ammonium chloride：42~52%, stirring and dissolving, add organic
Change porous diatomite：18~28%, it is well mixed, azo-bis-iso-dimethyl：2~5%, each component sum is percent
Hundred, it is washed with deionized water in 65 ± 2 DEG C of constant temperature, stirring, 6~8h of back flow reaction, separation of solid and liquid after cooling, the solid after separation
Wash, untill being washed till filtrate in neutrality, filter, dry, obtain the modified porous diatomite of dimethyl diallyl ammonium chloride.
2. according to the modified porous diatomaceous preparation method of a kind of dimethyl diallyl ammonium chloride described in claim 1,
Characterized in that, the filtrate described in step (3) after separation of solid and liquid adds the 3- chloropropyl front threes of 5~8% mass percents again
After TMOS, it can be continuing with.
3. according to the modified porous diatomaceous preparation method institute of a kind of dimethyl diallyl ammonium chloride described in claim 1
The modified porous diatomite of dimethyl diallyl ammonium chloride of preparation, it is characterised in that dimethyl diallyl ammonium chloride is modified
Porous diatomite adsorbant adsorbs to waste water Crude Oil, diesel oil, lubricating oil, vegetable oil, gasoline.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103709326A (en) * | 2013-12-27 | 2014-04-09 | 福建清源科技有限公司 | Preparation method of cationic organic silicon modified poly(diallyldimethylammonium chloride) fixing agent |
| CN104445553A (en) * | 2014-11-25 | 2015-03-25 | 神州华美（北京）科技有限公司 | Composite water purifying agent and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN103709326A (en) * | 2013-12-27 | 2014-04-09 | 福建清源科技有限公司 | Preparation method of cationic organic silicon modified poly(diallyldimethylammonium chloride) fixing agent |
| CN104445553A (en) * | 2014-11-25 | 2015-03-25 | 神州华美（北京）科技有限公司 | Composite water purifying agent and preparation method and application thereof |
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