CN107670653A - A kind of paper mill sludge fiber micropore oil suction compound and its preparation method and application - Google Patents
A kind of paper mill sludge fiber micropore oil suction compound and its preparation method and application Download PDFInfo
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- CN107670653A CN107670653A CN201711116383.9A CN201711116383A CN107670653A CN 107670653 A CN107670653 A CN 107670653A CN 201711116383 A CN201711116383 A CN 201711116383A CN 107670653 A CN107670653 A CN 107670653A
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- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/26—Synthetic macromolecular compounds
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28023—Fibres or filaments
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3271—Hydroxyamines
- C08G18/3278—Hydroxyamines containing at least three hydroxy groups
- C08G18/3281—Hydroxyamines containing at least three hydroxy groups containing three hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6648—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38
- C08G18/6655—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3225 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3271
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/007—Contaminated open waterways, rivers, lakes or ponds
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Abstract
The invention belongs to field of environment engineering technology, and in particular to a kind of paper mill sludge fiber micropore oil suction compound and its preparation method and application.The present invention is directed to the problems of the prior art, there is provided a kind of paper mill sludge fiber micropore oil suction compound and its preparation method and application.Paper mill sludge fiber micropore oil suction compound of the present invention, it is made up of sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers and foaming agent；Wherein the volume ratio of sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers and foaming agent is 22~35:36~50:9~12:15~20；Material of the present invention is material cheap and easy to get, and preparation method is easy.The oils leakage pollution occasion of burst large area or large volume is can be widely applied to, leakage scope can be drawn a circle to approve by injection molding rapid build strip, sheet oil suction band, or combine concrete, wooden unit, sandbag and quickly form oil suction dam body.3~10m3 of structure barrier tape can be molded in 5~15min.
Description
Technical field
The invention belongs to field of environment engineering technology, and in particular to a kind of paper mill sludge fiber micropore oil suction compound and its
Preparation method and application.
Background technology
The yield of paper mill sludge is big, complicated component, is difficult to handle, and huge contamination hazard is caused to ecological environment, is
The study hotspot and difficult point of field of Environment Protection in recent years.Paper mill sludge mainly includes：The virgin fibers production link in paper mill produces
Preliminary sludge, to deinked sludge caused by the deinking of reuse, paper mill sewage disposal end productses caused by two
The mixture of secondary sludge, wherein preliminary sludge and secondary sludge is also referred to as mixing sludge.The content of organics of paper mill sludge is
38%~51%, the macromolecule organics such as cellulose, hemicellulose and lignin and chemical papermaking additive etc. are mainly contained,
Fiber substance content therein accounts for the 27%~39% of sludge gross weight.The content of beary metal of its preliminary sludge and secondary sludge
It is relatively low, it is a kind of high-quality biomass resource, there is good recycling value.Conventional treatment method for paper mill sludge is
Landfill burns, and such method wastes good fiber quality cellulosic material therein.Handled according to composting process, it is first right to need again
Cellulose therein, which is implemented to break, surely to be pre-processed to improve its degradability, it is necessary to consume a large amount of soda acid chemical raw materials.
The core material of the present invention uses preliminary sludge and secondary sludge caused by paper industry, it is used different pre-
Handling process, its chemical modification is realized, make full use of the skeleton structure stability of sludge cellulose, carried for composite molding oil suction band
For cross-linking supports.Coordinate and the auxiliary materials such as Ji ﹑ foaming agents are Dinged with polyurethane Yu Ju Wu ﹑ Wen, by rapid shaping technique, form multiple
Oil suction band is closed, realizes the high efficiency absorption to oil pollutant.The oils that can be widely applied to burst large area or large volume is let out
Leakage pollution occasion, can quickly draw a circle to approve leakage scope, and disposing oil pollution accident for high efficiency provides novel emergency means.For enterprise
Industry safety in production, environmental and ecological protection have very high social value, and good market popularization value.
The content of the invention
The present invention is directed to the problems of the prior art, there is provided a kind of paper mill sludge fiber micropore oil suction compound and its preparation
Methods and applications.
The technical scheme is that：
A kind of paper mill sludge fiber micropore oil suction compound, by sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers and hair
Infusion forms；Wherein the volume ratio of sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers and foaming agent is 22~35:36~50:
9~12:15~20；
Wherein described sludge fiber master batch is to use preliminary sludge caused by paper industry with secondary sludge for raw material, warp
Cross fibre material extraction, desiccation preprocessing process obtains；
Described polyurethane prepolymer is prepared by the following method：Use PEPA (hydroxyl value for 310~
360mgKOH/g) with triethanolamine with volume ratio 1：0.08~0.12 ratio mixing, 1.5 are dehydrated under the conditions of 90~105 DEG C
~2.0 hours, after being down to room temperature, with toluene di-isocyanate(TDI) (2,4-TDI80%, 2,6-TDI20%) with volume ratio 1:1.2~
1.8 ratio mixing, progressively heats up and is reacted 1.5~2.0 hours under the conditions of 25~90 DEG C, after deaeration is handled, obtain poly- ammonia
Ester prepolymer.
As the preferred scheme of the present invention, the moisture content 65~73% of preliminary sludge of the present invention, content of cellulose 42
~53%.
As the present invention preferred scheme, the moisture content 72~78% of secondary sludge of the present invention, content of cellulose 35~
40%.
It is as follows as the preferred scheme of the present invention, the preparation method of sludge fiber master batch of the present invention：First by preliminary sludge with
Secondary sludge carries out high-speed stirred, and speed of agitator 240r/min, mixing time is 40~60s, makes preliminary sludge and secondary dirt
The viscosity of mud is decreased to less than 2900mPas；Then 1.0 that mass percent is preliminary sludge and secondary sludge gross mass are added
~1.5% sodium potassium tartrate tetrahydrate, then using rotary drum 1500~1700r/min of rotating speed, 1.5~2.0r/min of differential speed, remove thick
Matter inorganic matter, then 30~45min is dried at being 90~105 DEG C in temperature, it is prepared into sludge fiber master batch.
As the preferred scheme of the present invention, stabilizer of the invention is that mass ratio is 1：2.5~3.0 carboxymethyl cellulose
With the mixture of 4- methyhnorpholine-N-oxides.
As the preferred scheme of the present invention, foaming agent of the present invention is sodium dodecyl sulfate solution.
As the preferred scheme of the present invention, the mass percent of sodium dodecyl sulfate solution of the present invention for 20~
35%.
The preparation method of the composite microporous oil suction compound of rapid shaping of the present invention, comprises the following steps：
(1) sludge fiber master batch is prepared：Preliminary sludge and secondary sludge are first subjected to high-speed stirred, speed of agitator is
240r/min, mixing time are 40~60s, the viscosity of preliminary sludge and secondary sludge is decreased to less than 2900mPas；Then
It is preliminary sludge and 1.0~1.5% sodium potassium tartrate tetrahydrate of secondary sludge gross mass to add mass percent, then is turned using rotary drum
Speed 1500~1700r/min, 1.5~2.0r/min of differential speed, remove thick matter inorganic matter；Finally in the case where temperature is 90~105 DEG C
30~45min is dried, is prepared into sludge fiber master batch；
(2) polyurethane prepolymer is prepared：Use PEPA (hydroxyl value is 310~360mgKOH/g) and triethanolamine with
Volume ratio 1：0.08~0.12 ratio mixing, is dehydrated 1.5~2.0 hours under the conditions of 90~105 DEG C, after being down to room temperature, with
Toluene di-isocyanate(TDI) (2,4-TDI80%, 2,6-TDI20%) is with volume ratio 1:1.2~1.8 ratio mixing, progressively heats up
Reacted 1.5~2.0 hours under the conditions of 25~90 DEG C, after deaeration is handled, obtain polyurethane prepolymer；
(3) will be 1 according to mass ratio：2.5~3.0 ratio takes carboxymethyl cellulose and 4- methyhnorpholine-N-oxides
It is well mixed that stabilizer is made, it is 22~35 according still further to volume ratio:36~50:9~12 ratio is by sludge fiber master batch, poly- ammonia
Ester prepolymer is well mixed with stabilizer under the conditions of 75~80 DEG C；
(4) it is steady according to sludge fiber master batch, polyurethane Yu Ju Wu ﹑ using sodium dodecyl sulfate solution as foaming agent
The volume ratio for determining agent and foaming agent is 22~35:36~50:9~12:15~20 ratio takes sodium dodecyl sulfate solution to add
Enter in the material of step (3) gentle agitation under the conditions of 30~35 DEG C be well mixed at a slow speed with 30r/min rotating speed be made it is quick
It is molded composite microporous oil suction compound.
The application of the composite microporous oil suction compound of rapid shaping of the present invention, for quick adsorption oily substance, concrete application
Method is：The composite microporous oil suction compound of rapid shaping is loaded in the pressure-resistant inhalator jar of sealing, pressure when keeping 25 DEG C in tank
Power is 5~6kg/cm2, tank mouth sets switch and flow valve, after tank body switch is opened, rotary current valve regulation aerosol flow,
Sprayed to oil pollution object area, spray the fiber composite rich in foam, implement absorption, parcel to oil pollutant.
The invention has the advantages that：
1st, the present invention effectively plays the effect of sludge fibr tissue, realized using paper mill sludge as Core Feature material
The twice laid of sludge, new application idea is opened for Treatment of Sludge and disposal, belongs to new type resource comprehensive utilization technique.
Meanwhile the novel emergency material of convenient and efficient is provided for the emergency disposal of increasingly serious enterprise's oil pollution accident again, keep away
Exempt from contamination, ensure social stability.
2nd, the paper mill sludge fiber rapid shaping compound prepared by the present invention, is the bone using sludge fiber as mixture
Frame structure, it can play a part of assisting each composition crosslinking to combine, there is very strong stability.Improve composite system
Lipophile, it is poor to solve common blown polyurethane materials absorption property, it is impossible to be used in the greasy dirt absorption problem at the scene of polluting.Due to
The macromolecule organics such as cellulose, hemicellulose and lignin in its components utilising sludge, belong to " biodegradable fiber element base
Material ", degradability of the oil suction band after emergent accident disposal is enhanced, its environment friendly is enhanced, is advantageous to avoid inhaling
The secondary pollution hidden danger that oily band is brought after discarding to landfill yard to environment.After completing to the absorption of greasy dirt, due to its phase
To loose porous fibrous structure, it is easy to root out cleaning.If disposing these " waste materials " using burning method, its heat can be improved again
Value, improve the combustibility of material.
3rd, the composition such as polyurethane Yu Ju Wu ﹑ foaming agents of the present invention, stabilizer, a large amount of micropore bubbles can be generated
Foam, metastable loose structure is formed with sludge fiber composite.The bubble hole formed after injection be mainly diameter 1.0~
4.0mm micropore.This " fiber --- polyurethane --- bubble " composite construction enhances to be connect with oil pollution onsite surface
Touch binding ability；Before Emergency use, it is not required to carry out base treatment, is not required to clean out dust, greasy dirt of live contact layer etc.,
It is easy to use.There is realistic meaning to enterprise accident disposal and prevention and cure of pollution.
4th, material of the present invention is material cheap and easy to get, and preparation method is easy.It can be widely applied to happen suddenly
The oils leakage pollution occasion of large area or large volume, it can be let out by injection molding rapid build strip, sheet oil suction band, delineation
Scope is leaked, or combines concrete, wooden unit, sandbag and quickly forms oil suction dam body.It can be molded 3~10m3's of structure in 5~15min
Barrier tape.Both the pollution leakage that can be used for enterprise ground intercepts, and can be used for the oil pollution absorption in river lake water face again.It is beneficial to
Popularization and application, both belong to environmental pollution treatment technology, fall within a kind of new material technology of preparing.
Embodiment
Embodiment 1
A kind of paper mill sludge fiber micropore oil suction compound, by sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers and hair
Infusion forms；Wherein the volume ratio of sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers and foaming agent is 22:36:9:15；
The preparation method of wherein described sludge fiber master batch is as follows：Preliminary sludge and secondary sludge are first subjected to high-speed stirring
Mix, speed of agitator 240r/min, mixing time 40s, be decreased to less than the viscosity of preliminary sludge and secondary sludge
2900mPa·s；Then mass percent is added as preliminary sludge and 1.0% sodium potassium tartrate tetrahydrate of secondary sludge gross mass, then
Using rotary drum rotating speed 1500r/min, differential speed 1.5r/min, thick matter inorganic matter is removed, then dried at being 90 DEG C in temperature
30min, it is prepared into sludge fiber master batch.
Described polyurethane prepolymer is prepared by the following method：Use PEPA (hydroxyl value for 310~
360mgKOH/g) with triethanolamine with volume ratio 1：0.08 ratio mixing, is dehydrated 1.5 hours under the conditions of 90 DEG C, is down to room
Wen Hou, with toluene di-isocyanate(TDI) (2,4-TDI80%, 2,6-TDI20%) with volume ratio 1:1.2 ratio mixing, progressively rises
Temperature is reacted 1.5 hours under the conditions of 25 DEG C, after deaeration is handled, obtains polyurethane prepolymer；
Described foaming agent is the sodium dodecyl sulfate solution that mass percent is 20%；
The moisture content 65% of preliminary sludge described in the present embodiment, content of cellulose 42%.
The moisture content 72% of secondary sludge, content of cellulose 35% in the present embodiment.
Stabilizer described in the present embodiment is that mass ratio is 1：2.5 carboxymethyl cellulose and 4- methyl morpholine-N- oxygen
The mixture of compound.
The preparation method of the composite microporous oil suction compound of the present embodiment rapid shaping, comprises the following steps：
(1) sludge fiber master batch is prepared：Preliminary sludge and secondary sludge are first subjected to high-speed stirred, speed of agitator is
240r/min, mixing time 40s, the viscosity of preliminary sludge and secondary sludge is set to be decreased to less than 2900mPas；Then add
Mass percent is preliminary sludge and 1.0% sodium potassium tartrate tetrahydrate of secondary sludge gross mass, then using rotary drum rotating speed 1500r/
Min, differential speed 1.5r/min, remove thick matter inorganic matter；30min is dried at being finally 90 DEG C in temperature, is prepared into sludge fiber
Masterbatch；
(2) polyurethane prepolymer is prepared：Use PEPA (hydroxyl value is 310~360mgKOH/g) and triethanolamine with
Volume ratio 1：0.08 ratio mixing, be dehydrated 1.5 hours under the conditions of 90 DEG C, after being down to room temperature, with toluene di-isocyanate(TDI) (2,
4-TDI80%, 2,6-TDI20%) with volume ratio 1:1.2 ratio mixing, the reaction 1.5 under the conditions of 25 DEG C that progressively heats up are small
When, after deaeration is handled, obtain polyurethane prepolymer；
(3) will be 1 according to mass ratio：2.5 ratio takes carboxymethyl cellulose to be mixed with 4- methyhnorpholine-N-oxides
It is even that stabilizer is made, it is 22 according still further to volume ratio:36:9 ratio exists sludge fiber master batch, polyurethane prepolymer and stabilizer
It is well mixed under the conditions of 75 DEG C；
(4) it is steady according to sludge fiber master batch, polyurethane Yu Ju Wu ﹑ using sodium dodecyl sulfate solution as foaming agent
The volume ratio for determining agent and foaming agent is 22:36:9:15 ratio takes sodium dodecyl sulfate solution to add in the material of step (3)
Gentle agitation is well mixed at a slow speed that the composite microporous oil suction of rapid shaping is made is compound with 30r/min rotating speed under the conditions of 30 DEG C
Thing.
The present embodiment micropore oil suction compound is used for quick adsorption oily substance, and concrete application method is：By rapid shaping
Composite microporous oil suction compound is loaded in the pressure-resistant inhalator jar of sealing, and pressure when keeping 25 DEG C in tank is 5~6kg/cm2, tank
Mouth sets switch and flow valve, after tank body switch is opened, rotary current valve regulation aerosol flow, enters to oil pollution object area
Row injection, sprays the fiber composite rich in foam, implements absorption, parcel to oil pollutant.
Embodiment 2
A kind of paper mill sludge fiber micropore oil suction compound, by sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers and hair
Infusion forms；Wherein the volume ratio of sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers and foaming agent is 35:50:12:20；
The preparation method of wherein described sludge fiber master batch is as follows：Preliminary sludge and secondary sludge are first subjected to high-speed stirring
Mix, speed of agitator 240r/min, mixing time 60s, be decreased to less than the viscosity of preliminary sludge and secondary sludge
2900mPa·s；Then mass percent is added as preliminary sludge and 1.5% sodium potassium tartrate tetrahydrate of secondary sludge gross mass, then
Using rotary drum rotating speed 1700r/min, differential speed 2.0r/min, thick matter inorganic matter is removed, then dried at being 105 DEG C in temperature
45min, it is prepared into sludge fiber master batch.
Described polyurethane prepolymer is prepared by the following method：Use PEPA (hydroxyl value for 310~
360mgKOH/g) with triethanolamine with volume ratio 1：0.12 ratio mixing, is dehydrated 2.0 hours under the conditions of 105 DEG C, is down to room
Wen Hou, with toluene di-isocyanate(TDI) (2,4-TDI80%, 2,6-TDI20%) with volume ratio 1:1.8 ratio mixing, progressively rises
Temperature is reacted 2.0 hours under the conditions of 90 DEG C, after deaeration is handled, obtains polyurethane prepolymer；
Described foaming agent is the sodium dodecyl sulfate solution that mass percent is 35%；
The moisture content 73% of preliminary sludge described in the present embodiment, content of cellulose 53%.
The moisture content 78% of secondary sludge, content of cellulose 40% in the present embodiment.
Stabilizer described in the present embodiment is that mass ratio is 1：3.0 carboxymethyl cellulose and 4- methyl morpholine-N- oxygen
The mixture of compound.
The preparation method of the present embodiment paper mill sludge fiber micropore oil suction compound, comprises the following steps：
(1) sludge fiber master batch is prepared：Preliminary sludge and secondary sludge are first subjected to high-speed stirred, speed of agitator is
240r/min, mixing time 60s, the viscosity of preliminary sludge and secondary sludge is set to be decreased to less than 2900mPas；Then add
Mass percent is preliminary sludge and 1.5% sodium potassium tartrate tetrahydrate of secondary sludge gross mass, then using rotary drum rotating speed 1700r/
Min, differential speed 2.0r/min, remove thick matter inorganic matter；45min is dried at being finally 105 DEG C in temperature, is prepared into sludge fiber
Masterbatch；
(2) polyurethane prepolymer is prepared：Use PEPA (hydroxyl value is 310~360mgKOH/g) and triethanolamine with
The ratio mixing of volume ratio 1: 0.12, is dehydrated 2.0 hours under the conditions of 105 DEG C, after being down to room temperature, with toluene di-isocyanate(TDI)
(2,4-TDI80%, 2,6-TDI20%) are with volume ratio 1:1.8 ratio mixing, progressively heats up and reacts 2.0 under the conditions of 90 DEG C
Hour, after deaeration is handled, obtain polyurethane prepolymer；
(3) according to the ratio that mass ratio is 1: 3.0 carboxymethyl cellulose will be taken to be mixed with 4- methyhnorpholine-N-oxides
It is even that stabilizer is made, it is 35 according still further to volume ratio:50:12 ratio is by sludge fiber master batch, polyurethane prepolymer and stabilizer
It is well mixed under the conditions of 80 DEG C；
(4) it is steady according to sludge fiber master batch, polyurethane Yu Ju Wu ﹑ using sodium dodecyl sulfate solution as foaming agent
The volume ratio for determining agent and foaming agent is 35:50:12:20 ratio takes the material of sodium dodecyl sulfate solution addition step (3)
In under the conditions of 30~35 DEG C gentle agitation with 30r/min rotating speed at a slow speed be well mixed the composite microporous oil suction of rapid shaping is made
Compound.
The present embodiment paper mill sludge fiber micropore oil suction compound is used for quick adsorption oily substance, concrete application method
For：The composite microporous oil suction compound of rapid shaping is loaded in the pressure-resistant inhalator jar of sealing, it is 5 that pressure at 25 DEG C is kept in tank
~6kg/cm2, tank mouth sets switch and flow valve, after tank body switch is opened, rotary current valve regulation aerosol flow, to oils
Pollution object area is sprayed, and sprays the fiber composite rich in foam, implements absorption, parcel to oil pollutant.
Embodiment 3
A kind of paper mill sludge fiber micropore oil suction compound, by sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers and hair
Infusion forms；Wherein the volume ratio of sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers and foaming agent is 30:45:10:18；
The preparation method of wherein described sludge fiber master batch is as follows：Preliminary sludge and secondary sludge are first subjected to high-speed stirring
Mix, speed of agitator 240r/min, mixing time 50s, be decreased to less than the viscosity of preliminary sludge and secondary sludge
2900mPa·s；Then mass percent is added as preliminary sludge and 1.2% sodium potassium tartrate tetrahydrate of secondary sludge gross mass, then
Using rotary drum rotating speed 1600r/min, differential speed 1.8r/min, thick matter inorganic matter is removed, then dried at being 98 DEG C in temperature
40min, it is prepared into sludge fiber master batch.
Described polyurethane prepolymer is prepared by the following method：Use PEPA (hydroxyl value for 310~
360mgKOH/g) with triethanolamine with volume ratio 1：0.1 ratio mixing, is dehydrated 1.6 hours under the conditions of 98 DEG C, is down to room temperature
Afterwards, with toluene di-isocyanate(TDI) (2,4-TDI80%, 2,6-TDI20%) with volume ratio 1:1.6 ratio mixing, progressively heats up
Reacted 1.6 hours under the conditions of 50 DEG C, after deaeration is handled, obtain polyurethane prepolymer；
Described foaming agent is the sodium dodecyl sulfate solution that mass percent is 25%；
The moisture content 70% of preliminary sludge described in the present embodiment, content of cellulose 48%.
The moisture content 75% of secondary sludge, content of cellulose 38% in the present embodiment.
Stabilizer described in the present embodiment is that mass ratio is 1：2.7 carboxymethyl cellulose and 4- methyl morpholine-N- oxygen
The mixture of compound.
The preparation method of the present embodiment paper mill sludge fiber micropore oil suction compound, comprises the following steps：
(1) sludge fiber master batch is prepared：Preliminary sludge and secondary sludge are first subjected to high-speed stirred, speed of agitator is
240r/min, mixing time 50s, the viscosity of preliminary sludge and secondary sludge is set to be decreased to less than 2900mPas；Then add
Mass percent is preliminary sludge and 1.2% sodium potassium tartrate tetrahydrate of secondary sludge gross mass, then using rotary drum rotating speed 1600r/
Min, differential speed 1.8r/min, remove thick matter inorganic matter；40min is dried at being finally 98 DEG C in temperature, is prepared into sludge fiber
Masterbatch；
(2) polyurethane prepolymer is prepared：Use PEPA (hydroxyl value is 310~360mgKOH/g) and triethanolamine with
Volume ratio 1：0.1 ratio mixing, be dehydrated 1.6 hours under the conditions of 98 DEG C, after being down to room temperature, with toluene di-isocyanate(TDI) (2,
4-TDI80%, 2,6-TDI20%) with volume ratio 1:1.5 ratio mixing, the reaction 1.6 under the conditions of 50 DEG C that progressively heats up are small
When, after deaeration is handled, obtain polyurethane prepolymer；
(3) will be 1 according to mass ratio：2.8 ratio takes carboxymethyl cellulose to be mixed with 4- methyhnorpholine-N-oxides
It is even that stabilizer is made, it is 30 according still further to volume ratio:45:10 ratio is by sludge fiber master batch, polyurethane prepolymer and stabilizer
It is well mixed under the conditions of 78 DEG C；
(4) it is steady according to sludge fiber master batch, polyurethane Yu Ju Wu ﹑ using sodium dodecyl sulfate solution as foaming agent
The volume ratio for determining agent and foaming agent is 30:45:10:18 ratio takes the material of sodium dodecyl sulfate solution addition step (3)
In under the conditions of 32 DEG C gentle agitation be well mixed that the composite microporous oil suction of rapid shaping is made is compound at a slow speed with 30r/min rotating speed
Thing.
The present embodiment paper mill sludge fiber micropore oil suction compound is used for quick adsorption oily substance, concrete application method
For：The composite microporous oil suction compound of rapid shaping is loaded in the pressure-resistant inhalator jar of sealing, it is 5 that pressure at 25 DEG C is kept in tank
~6kg/cm2, tank mouth sets switch and flow valve, after tank body switch is opened, rotary current valve regulation aerosol flow, to oils
Pollution object area is sprayed, and sprays the fiber composite rich in foam, implements absorption, parcel to oil pollutant.
Claims (10)
- A kind of 1. paper mill sludge fiber micropore oil suction compound, it is characterized in that stable by sludge fiber master batch, polyurethane Yu Ju Wu ﹑ Agent and foaming agent composition；Wherein the volume ratio of sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers and foaming agent is 22~35: 36~50:9~12:15~20；Wherein described sludge fiber master batch is to use preliminary sludge caused by paper industry with secondary sludge for raw material, by fibre Tie up material extraction, desiccation preprocessing process obtains；Described polyurethane prepolymer is prepared by the following method：Use PEPA (hydroxyl value for 310~ 360mgKOH/g) with triethanolamine with volume ratio 1：0.08~0.12 ratio mixing, 1.5 are dehydrated under the conditions of 90~105 DEG C ~2.0 hours, after being down to room temperature, with toluene di-isocyanate(TDI) (2,4-TDI80%, 2,6-TDI20%) with volume ratio 1:1.2~ 1.8 ratio mixing, progressively heats up and is reacted 1.5~2.0 hours under the conditions of 25~90 DEG C, after deaeration is handled, obtain poly- ammonia Ester prepolymer.
- A kind of 2. paper mill sludge fiber micropore oil suction compound according to claim 1, it is characterized in that the preliminary sludge Moisture content 65~73%, content of cellulose 42~53%.
- A kind of 3. paper mill sludge fiber micropore oil suction compound according to claim 1, it is characterized in that the secondary sludge Moisture content 72~78%, content of cellulose 35~40%.
- A kind of 4. paper mill sludge fiber micropore oil suction compound according to claim 1, it is characterized in that the sludge fiber The preparation method of masterbatch is as follows：Preliminary sludge and secondary sludge are first subjected to high-speed stirred, speed of agitator 240r/min, stirring Time is 40~60s, the viscosity of preliminary sludge and secondary sludge is decreased to less than 2900mPas；Then mass percent is added For 1.0~1.5% sodium potassium tartrate tetrahydrate of preliminary sludge and secondary sludge gross mass, then using 1500~1700r/ of rotary drum rotating speed Min, 1.5~2.0r/min of differential speed, thick matter inorganic matter is removed, then 30~45min, system are dried at being 90~105 DEG C in temperature It is standby into sludge fiber master batch.
- A kind of 5. paper mill sludge fiber micropore oil suction compound according to claim 1, it is characterized in that described stabilizer It is 1 for mass ratio：2.5~3.0 carboxymethyl cellulose and the mixture of 4- methyhnorpholine-N-oxides.
- A kind of 6. paper mill sludge fiber micropore oil suction compound according to claim 1, it is characterized in that described foaming agent For sodium dodecyl sulfate solution.
- A kind of 7. paper mill sludge fiber micropore oil suction compound according to claim 6, it is characterized in that described dodecane The mass percent of base metabisulfite solution is 20~35%.
- 8. a kind of preparation method of paper mill sludge fiber micropore oil suction compound of any one in claim 1-7, it is characterized in that Comprise the following steps：(1) sludge fiber master batch is prepared：Preliminary sludge and secondary sludge are first subjected to high-speed stirred, speed of agitator 240r/ Min, mixing time are 40~60s, the viscosity of preliminary sludge and secondary sludge is decreased to less than 2900mPas；Then matter is added It is preliminary sludge and 1.0~1.5% sodium potassium tartrate tetrahydrate of secondary sludge gross mass to measure percentage, then using rotary drum rotating speed 1500 ~1700r/min, 1.5~2.0r/min of differential speed, remove thick matter inorganic matter；30 are dried at being finally 90~105 DEG C in temperature ~45min, it is prepared into sludge fiber master batch；(2) polyurethane prepolymer is prepared：Use PEPA (hydroxyl value is 310~360mgKOH/g) with triethanolamine with volume Ratio mixing than 1: 0.08~0.12, is dehydrated 1.5~2.0 hours under the conditions of 90~105 DEG C, after being down to room temperature, with toluene Diisocyanate (2,4-TDI80%, 2,6-TDI20%) is with volume ratio 1:1.2~1.8 ratio mixing, progressively heats up in 25 Reacted 1.5~2.0 hours under the conditions of~90 DEG C, after deaeration is handled, obtain polyurethane prepolymer；(3) will be 1 according to mass ratio：2.5~3.0 ratio takes carboxymethyl cellulose to be mixed with 4- methyhnorpholine-N-oxides Stabilizer uniformly is made, is 22~35 according still further to volume ratio:36~50:9~12 ratio is pre- by sludge fiber master batch, polyurethane Polymers is well mixed with stabilizer under the conditions of 75~80 DEG C；(4) using sodium dodecyl sulfate solution as foaming agent, according to sludge fiber master batch, polyurethane Yu Ju Wu ﹑ stabilizers Volume ratio with foaming agent is 22~35:36~50:9~12:15~20 ratio takes sodium dodecyl sulfate solution to add step Suddenly rapid shaping is made so that 30r/min rotating speed is well mixed at a slow speed in gentle agitation under the conditions of 30~35 DEG C in the material of (3) Composite microporous oil suction compound.
- A kind of 9. application of paper mill sludge fiber micropore oil suction compound of any one in claim 1-7, it is characterized in that being used for Quick adsorption oily substance.
- A kind of 10. application of paper mill sludge fiber micropore oil suction compound according to claim 9, it is characterized in that will be quick Absorption oily substance concrete application method be：The composite microporous oil suction compound of rapid shaping is loaded on the pressure-resistant inhalator jar of sealing In, pressure when keeping 25 DEG C in tank is 5~6kg/cm2, tank mouth sets switch and flow valve, after tank body switch is opened, rotation Turn of tidal stream amount valve regulation aerosol flow, is sprayed to oil pollution object area, the fiber composite rich in foam is sprayed, to oils Pollutant implements absorption, parcel.
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