CN105642237B - A kind of preparation method of endecatylene amido propyl betaine modification infusorial earth - Google Patents
A kind of preparation method of endecatylene amido propyl betaine modification infusorial earth Download PDFInfo
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- CN105642237B CN105642237B CN201610087645.2A CN201610087645A CN105642237B CN 105642237 B CN105642237 B CN 105642237B CN 201610087645 A CN201610087645 A CN 201610087645A CN 105642237 B CN105642237 B CN 105642237B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/14—Diatomaceous earth
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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Abstract
The invention discloses a kind of preparation method of endecatylene amido propyl betaine modification infusorial earth, it is characterised in that after diatomite is handled with 2mol/L HCl, obtains pre-processing diatomite；Pretreatment diatomite is organised with absolute ethyl alcohol and 3 r-chloropropyl trimethoxyl silanes；Then, in the reactor, deionized water is added by following composition mass percent：45 ~ 55%, endecatylene amido propyl betaine：8 ~ 18%, stirring and dissolving, add the diatomite that organises：28 ~ 38%, it is well mixed, adds the hydrogen peroxide that mass percentage concentration is 30%：5 ~ 8%, each component sum is a hundred per cent, in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 4 ~ 6, separation of solid and liquid after cooling, the solid after separation are washed with deionized, untill being washed till filtrate in neutrality, filtering, dry, obtain endecatylene amido propyl betaine modification infusorial earth.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 preparation method of more particularly to a kind of endecatylene amido propyl betaine modification infusorial earth and its answering in water process
With.
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
The water that chemical modification prepares a kind of material of oil suction and is used for sewage is carried out to diatomite using endecatylene amido propyl betaine
In processing, diatomaceous new application is developed.
Endecatylene amido propyl betaine, pale yellow transparent thick liquid is soluble in water, has excellent performance, pole
The amphoteric surfactant of low irritant, this product are a kind of bifunctional compounds, containing alkyl functional group and amido functionality,
With excellent oil absorbency.The material being modified with endecatylene amido propyl betaine has very strong lipophile, is fine
Oil absorption material.
Through retrieval, the preparation method using endecatylene amido propyl betaine modification infusorial earth is had no, and applied
The oily absorption report into sewage disposal.
The content of the invention
An object of the present invention is to provide a kind of preparation method of endecatylene amido propyl betaine modification infusorial earth,
Another object is that the endecatylene amido propyl betaine modification infusorial earth of preparation is applied in wastewater treatment as adsorbent.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of endecatylene amido propyl betaine modification infusorial earth, it is characterised in that this method have with
Lower processing step：
（1）Diatomaceous pretreatment：Sieve by diatomite with 140 mesh, it is 1g by solid-to-liquid ratio：3mL, by diatom
Soil is added in 2mol/L HCl/water solution, and temperature rises to 80 ~ 90 DEG C, the min of stirring reaction 30 ~ 40, after cooling, filtering, uses water
Washing is dried to neutrality, obtains pre-processing diatomite；
（2）Organise diatomite：In the reactor, added by following composition mass percent：Absolute ethyl alcohol：46 ~ 56%,
3- r-chloropropyl trimethoxyl silanes：16 ~ 26%, stirring and dissolving, add pretreatment 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 diatomite that organises；
（3）Endecatylene amido propyl betaine modification infusorial earth preparation method：In the reactor, by following composition quality
Percentage adds deionized water：45 ~ 55%, endecatylene amido propyl betaine：8 ~ 18%, stirring and dissolving, add and organise
Diatomite：28 ~ 38%, it is well mixed, adds the hydrogen peroxide that mass percentage concentration is 30%：5 ~ 8%, each component sum is percentage
Hundred, be washed with deionized water in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 4 ~ 6, separation of solid and liquid after cooling, the solid after separation
Wash, untill being washed till filtrate in neutrality, filter, dry, obtain endecatylene amido propyl betaine modification infusorial earth.
Step（2）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.
Step（3）Described in filtrate after separation of solid and liquid add the endecatylene amido propyl sweet teas of 2 ~ 5% mass percents again
After dish alkali, it can be continuing with.
It is a further object of the present invention to provide using the endecatylene amido propyl betaine modification infusorial earth of preparation as suction
Attached dose is applied to grease in waste water and handles, 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 endecatylene amido propyl betaine modified silicon that will be prepared
Diatomaceous earth soaks 1 ~ 2h with deionized water, is adsorbed by static method；Adsorbed by dynamic method, adsorbent is loaded into adsorption column, it is grease-contained
Waste water passes through by 6.0 mL/min of flow velocity.
Advantages of the present invention and effect are：
（1）The endecatylene amido propyl betaine modification infusorial earth that the present invention obtains has good physical chemistry stable
Property and excellent mechanical strength, adsorption capacity are big, and maximum adsorption capacity 221.5mg/g, Reusability number is up to more than 10 times；
（2）The endecatylene amido propyl betaine modification infusorial earth that the present invention obtains is to various greases in water body（Such as original
Oil, diesel oil, lubricating oil, machine oil, vegetable oil, gasoline etc.）There are preferably absorption and elution, adsorption efficiency is high, and the speed of absorption is fast,
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.
(4) waste liquid of building-up process is reusable, three-waste free discharge, environmental protection.
Embodiment
Embodiment 1
（1）Diatomaceous pretreatment：Sieve by diatomite with 140 mesh, it is 1g by solid-to-liquid ratio：3mL, by diatom
Soil is added in 2mol/L HCl/water solution, and temperature rises to 85 DEG C, the min of stirring reaction 35, after cooling, filtering, is washed with water to
Neutrality, dry, obtain pre-processing diatomite；
（2）Organise diatomite：In the reactor, it is separately added into：Absolute ethyl alcohol：63 mL, 3- r-chloropropyl trimethoxyl
Silane：20g, stirring and dissolving, add pretreatment diatomite：30g, temperature rise to 55 DEG C, the h of back flow reaction 7, after cooling, solid-liquid
Separation, the solid after separation are washed with deionized, and untill being washed till filtrate in neutrality, dry, obtain the diatomite that organises；
（3）Endecatylene amido propyl betaine modification infusorial earth preparation method：In the reactor, it is separately added into deionization
Water：50mL, endecatylene amido propyl betaine：13g, stirring and dissolving, add the diatomite that organises：31g, it is well mixed,
Add the hydrogen peroxide that mass percentage concentration is 30%：6 mL, it is solid after cooling in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 5
Liquid separates, and the solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, filters, dries, obtain endecatylene acyl
Amine CAB modification infusorial earth.
Embodiment 2
（1）Diatomaceous pretreatment：Sieve by diatomite with 140 mesh, it is 1g by solid-to-liquid ratio：3mL, by diatom
Soil is added in 2mol/L HCl/water solution, and temperature rises to 80 DEG C, stirring reaction 40min, after cooling, filtering, is washed with water to
Neutrality, dry, obtain pre-processing diatomite；
（2）Organise diatomite：In the reactor, it is separately added into：Absolute ethyl alcohol：70 mL, 3- r-chloropropyl trimethoxyl
Silane：16g, stirring and dissolving, add pretreatment diatomite：28g, temperature rise to 50 DEG C, the h of back flow reaction 8, after cooling, solid-liquid
Separation, the solid after separation are washed with deionized, and untill being washed till filtrate in neutrality, dry, obtain the diatomite that organises；
（3）Endecatylene amido propyl betaine modification infusorial earth preparation method：In the reactor, it is separately added into deionization
Water：55mL, endecatylene amido propyl betaine：12g, stirring and dissolving, add the diatomite that organises：28g, it is well mixed,
Add the hydrogen peroxide that mass percentage concentration is 30%：5 mL, it is solid after cooling in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 4
Liquid separates, and the solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, filters, dries, obtain endecatylene acyl
Amine CAB modification infusorial earth.
Embodiment 3
（1）Diatomaceous pretreatment：Sieve by diatomite with 140 mesh, it is 1g by solid-to-liquid ratio：3mL, by diatom
Soil is added in 2mol/L HCl/water solution, and temperature rises to 90 DEG C, the min of stirring reaction 33, after cooling, filtering, is washed with water to
Neutrality, dry, obtain pre-processing diatomite；
（2）Organise diatomite：In the reactor, it is separately added into：Absolute ethyl alcohol：58 mL, 3- r-chloropropyl trimethoxyl
Silane：22g, stirring and dissolving, add pretreatment diatomite：32g, temperature rise to 60 DEG C, back flow reaction 6h, after cooling, solid-liquid
Separation, the solid after separation are washed with deionized, and untill being washed till filtrate in neutrality, dry, obtain the diatomite that organises；
（3）Endecatylene amido propyl betaine modification infusorial earth preparation method：In the reactor, it is separately added into deionization
Water：45mL, endecatylene amido propyl betaine：10g, stirring and dissolving, add the diatomite that organises：38g, it is well mixed,
Add the hydrogen peroxide that mass percentage concentration is 30%：7 mL, in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 4.5, after cooling
Separation of solid and liquid, the solid after separation are washed with deionized, and untill being washed till filtrate in neutrality, filter, dry, obtain endecatylene
Amido propyl betaine modification infusorial earth.
Embodiment 4
（1）Diatomaceous pretreatment：Sieve by diatomite with 140 mesh, it is 1g by solid-to-liquid ratio：3mL, by diatom
Soil is added in 2mol/L HCl/water solution, and temperature rises to 85 DEG C, the min of stirring reaction 30, after cooling, filtering, is washed with water to
Neutrality, dry, obtain pre-processing diatomite；
（2）Organise diatomite：In the reactor, it is separately added into：Absolute ethyl alcohol：65 mL, 3- r-chloropropyl trimethoxyl
Silane：26g, stirring and dissolving, add pretreatment diatomite：22g, temperature rise to 58 DEG C, the h of back flow reaction 6.5, after cooling, Gu
Liquid separates, and the solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, dries, obtains the diatomite that organises；
（3）Endecatylene amido propyl betaine modification infusorial earth preparation method：In the reactor, it is separately added into deionization
Water：48mL, endecatylene amido propyl betaine：9g, stirring and dissolving, add the diatomite that organises：35g, it is well mixed, then
Add the hydrogen peroxide that mass percentage concentration is 30%：8 mL, it is solid after cooling in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 5.5
Liquid separates, and the solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, filters, dries, obtain endecatylene acyl
Amine CAB modification infusorial earth.
Embodiment 5
（1）Diatomaceous pretreatment：Sieve by diatomite with 140 mesh, it is 1g by solid-to-liquid ratio：3mL, by diatom
Soil is added in 2mol/L HCl/water solution, and temperature rises to 80 DEG C, the min of stirring reaction 40, after cooling, filtering, is washed with water to
Neutrality, dry, obtain pre-processing diatomite；
（2）Organise diatomite：In the reactor, it is separately added into：Absolute ethyl alcohol：68 mL, 3- r-chloropropyl trimethoxyl
Silane：21g, stirring and dissolving, add pretreatment diatomite：25g, temperature rise to 52 DEG C, the h of back flow reaction 7.5, after cooling, Gu
Liquid separates, and the solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, dries, obtains the diatomite that organises；
（3）Endecatylene amido propyl betaine modification infusorial earth preparation method：In the reactor, it is separately added into deionization
Water：45mL, endecatylene amido propyl betaine：18g, stirring and dissolving, add the diatomite that organises：30g, it is well mixed,
Add the hydrogen peroxide that mass percentage concentration is 30%：7 mL, it is solid after cooling in 65 ± 2 DEG C of constant temperature, stirring, the h of back flow reaction 5
Liquid separates, and the solid after separation is washed with deionized, and untill being washed till filtrate in neutrality, filters, dries, obtain endecatylene acyl
Amine CAB modification infusorial earth.
Embodiment 6
Weigh 0.50g endecatylene amido propyl betaine modification infusorial earth sorbing materials and be placed in 250mL conical flask with cover
In, adding 100mL concentration is in 550mg/L machine oil solution, using the pH value of acid or alkali regulation system as in the range of 5.0 ~ 10, in room
Lower concussion 1 ~ 2 h of absorption of temperature, takes supernatant, concentration oily in solution is determined with infrared spectrum oil content analyzer, according to water before and after absorption
Middle oily concentration difference, the adsorption capacity of endecatylene amido propyl betaine modification infusorial earth is calculated, its adsorption capacity highest
It can reach 221.5mg/g, pH value adsorbent in the range of 5.5 ~ 7.5 is maximum to the adsorption capacity of oil and stably, at room temperature
Concussion absorption more than 0.5h, absorption of the adsorbent to oil reach saturation.
Embodiment 7
Weigh 1.0g endecatylene amido propyl betaine modification infusorial earths to be placed in 250mL conical flask with cover, add
100mL concentration is in 100mg/L solution containing machine oil, and using the pH value of acid or alkali regulation system as 6.5, concussion at room temperature adsorbs 1
H, supernatant is taken, concentration oily in solution is determined with infrared spectrum oil content analyzer, according to concentration difference oily in water before and after absorption, calculated
Go out clearance of the octadecenamide CAB modification infusorial earth to oil, reach as high as 98.6%.
Claims (2)
- A kind of 1. preparation method of endecatylene amido propyl betaine modification infusorial earth, it is characterised in that this method have with Lower processing step：(1) diatomaceous pretreatment：Sieve by diatomite with 140 mesh, it is 1g by solid-to-liquid ratio：3mL, diatomite is added Into 2mol/L HCl/water solution, temperature rises to 80~90 DEG C, 30~40min of stirring reaction, after cooling, filtering, is washed with water To neutrality, dry, obtain pre-processing diatomite；(2) organise diatomite：In the reactor, added by following composition mass percent：Absolute ethyl alcohol：46~56%, 3- R-chloropropyl trimethoxyl silane：16~26%, stirring and dissolving, add pretreatment diatomite：22~32%, each component sum is Absolutely, temperature rises to 50~60 DEG C, 6~8h of back flow reaction, after cooling, separation of solid and liquid, the solid deionization after separation Water washing, untill being washed till filtrate in neutrality, dry, obtain the diatomite that organises；(3) endecatylene amido propyl betaine modification infusorial earth preparation method：In the reactor, by following composition quality percentage Than adding deionized water：45~55%, endecatylene amido propyl betaine：8~18%, stirring and dissolving, add and organise Diatomite：28~38%, it is well mixed, adds the hydrogen peroxide that mass percentage concentration is 30%：5~8%, each component sum is Absolutely, in 65 ± 2 DEG C of constant temperature, stirring, 4~6h of back flow reaction, separation of solid and liquid after cooling, the solid deionization after separation Water washing, untill being washed till filtrate in neutrality, filter, dry, obtain endecatylene amido propyl betaine modification infusorial earth.
- It is 2. made according to a kind of preparation method of endecatylene amido propyl betaine modification infusorial earth described in claim 1 Standby endecatylene amido propyl betaine modification infusorial earth, it is characterised in that endecatylene amido propyl betaine modified silicon Diatomaceous earth adsorbent adsorbs to waste water Crude Oil, diesel oil, lubricating oil, vegetable oil, gasoline.
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