CN105016860A - Production method of organic/inorganic composite magnetic-carried suspending agent - Google Patents

Production method of organic/inorganic composite magnetic-carried suspending agent Download PDF

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CN105016860A
CN105016860A CN201510382157.XA CN201510382157A CN105016860A CN 105016860 A CN105016860 A CN 105016860A CN 201510382157 A CN201510382157 A CN 201510382157A CN 105016860 A CN105016860 A CN 105016860A
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ommt
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CN105016860B (en
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刘志勇
吴建宁
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Abstract

The invention relates to a production method of an organic/inorganic composite magnetic-carried suspending agent, which comprises the following steps: 1)acidifying sodium-based montmorillonite (Na-MMT); 2)preparing a polyethylene glycol (PEG) solution intercalation Na-MMT; and 3)carrying organo montmorillonite (OMMT) on ferriferrous oxide (Fe3O4) to prepare the organic/inorganic composite magnetic-carried suspending agent. According to the invention, magnetic property of Fe3O4 is used for magnetizing water to improve the performance of the suspending agent, the method has the following characteristics that 1)PEG enables intercalation into interlayer of Na-MMT through a solution intercalation method, dispersibility and bonding force of Na-MMT in an organic matter are increased; 2)the Fe3O4 particles are carried in PEG-modified montmorillonite through a coprecipitation method, carrying is form, and magnetic performance is provided; and 3)bentonite resource in Xinjiang is abundant and has the advantage of low cost. The performance of the suspending agent is improved by introducing PEG and Fe3O4 particles.

Description

Organo-mineral complexing magnetic carries the production method of suspension agent
Technical field
The present invention relates to the production method that a kind of organo-mineral complexing magnetic carries suspension agent.
Background technology
China is a large agricultural country, mainly relies on water conservancy irrigation at present, and NORTHWEST CHINA area drought and water shortage, water is the most rare resources in these areas.Along with economic society is fast-developing, water resources disparities between supply and demand become increasingly conspicuous, and economize on water imperative; Since twentieth century the mid-90, Xinjiang big area under rare water resources induction have selected efficient water-saving irrigation technology, has now become agricultural high-effiency water-saving irrigation technique demonstration area domestic and the biggest in the world.Thus, liquid drip irrigation fertilizer arises at the historic moment, and in liquid drip irrigation fertilizer, suspension agent is very important auxiliary agent.Suspension agent has many good qualities, as without dust, easily mixing, improving suspensibility when diluting, improving wetting, lower packaging volume and strengthening biologicak efficiency; At present, suspension agent is mainly used in the fields such as agricultural chemicals, and the application in liquid drip irrigation fertilizer seldom has report, and the present invention utilizes Fe 3o 4load organo montmorillonite is prepared magnetic and is carried suspension agent and be applied in liquid drip irrigation fertilizer, by experiment, finds that this method can improve the performance of suspension agent, thus adds the utilization ratio of fertilizer.
Summary of the invention
The object of this invention is to provide the production method that a kind of performance is good, price is low organo-mineral complexing magnetic carries suspension agent.
The object of the invention is to be achieved through the following technical solutions:
Its feature of the present invention is: (the thing amount " part " of getting is weight part)
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Take the Na-MMT of 50 ~ 100 parts, 2 ~ 3h is dried under 100 ~ 120 DEG C of conditions, cross 200 ~ 300 mesh sieve, add in reactor, then add the hydrochloric acid soln of 0.5 ~ 2mol/L that 10 ~ 50 parts prepare, mechanical stirring 2 ~ 4h under 25 DEG C of conditions, leave standstill 24 ~ 36h, again supernatant liquor is poured out, be suspended thing 6 ~ 10 times by washed with de-ionized water, then by Na-MMT centrifugal 30 ~ 40min on the whizzer of 3000 ~ 10000rpm.After end, throw out is dried under 100 ~ 120 DEG C of conditions, grinding, crosses 200 ~ 300 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 50 ~ 100: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 0.5 ~ 2.5h, mechanical stirring 1 ~ 3h under 50 ~ 80 DEG C of conditions.Then slowly PEG2000 ~ 4000 are added according to Na-MMT: PEG mass ratio 1: 0.05 ~ 0.4, stirring velocity is promoted to 1000 ~ 1500rpm, continue reaction 2 ~ 4h, vacuum-drying 5 ~ 24h is carried out under 40 ~ 80 DEG C of conditions, grinding, cross 200 ~ 300 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 50 ~ 100 parts and 2000 ~ 6000 parts of deionized waters, then add 10 ~ 130 parts of FeCl 36H 2o is dissolved in deionized water, under 70 ~ 80 DEG C of conditions, stir 1 ~ 2h;
(2) again by 2 ~ 80 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 2 ~ 4mol/L, until stop when pH is 11 dripping, then reacts 2 ~ 5h.Reaction terminates rear washed with de-ionized water throw out 5 ~ 7 times, leaves standstill 12 ~ 24h, then is poured out by supernatant liquor, continue to use washed with de-ionized water 3 ~ 4 times, then use washes of absolute alcohol 3 ~ 4 times, under 40 ~ 80 DEG C of conditions, carry out vacuum drying, grinding, crosses 200 ~ 300 mesh sieve, obtains Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 4 ~ 12 (mass ratioes) with water, stirs 4 ~ 6h, obtain organo-mineral complexing magnetic and carry suspension agent under 85 ~ 90 DEG C of conditions.
Compared with prior art, the present invention utilizes Fe 3o 4magnetic by magnetic water, to improve the performance of suspension agent, feature is: PEG is intercalation into Na-MMT interlayer by solution intercalation method by (1), thus improves the dispersiveness of Na-MMT in organism and bonding force; (2) by coprecipitation method by Fe 3o 4particle load is in PEG modified montmorillonoid, and load is firm, has magnetic; (3) Xinjiang bentonite aboundresources, low price; This synthetic method is by introducing PEG and Fe 3o 4particle, improves the performance of suspension agent.
Embodiment
Embodiment 1:
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Take the Na-MMT of 50 parts, 2h is dried under 100 DEG C of conditions, cross 200 mesh sieve, add in reactor, then add the hydrochloric acid soln of the 0.5mol/L that 10 parts prepare, mechanical stirring 2h under 25 DEG C of conditions, leave standstill 24h, again supernatant liquor is poured out, be suspended thing 6 times by washed with de-ionized water, then by Na-MMT centrifugal 30min on the whizzer of 3000rpm.After end, throw out is dried under 100 DEG C of conditions, grinding, crosses 200 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 50: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 0.5h, mechanical stirring 1h under 50 DEG C of conditions; Then slowly add PEG2000 according to Na-MMT: PEG mass ratio 1: 0.05, stirring velocity is promoted to 1000rpm, continues reaction 2h, under 40 DEG C of conditions, carry out vacuum-drying 5h, grinding, cross 200 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 50 parts and 2000 parts of deionized waters, then add 10 parts of FeCl 36H 2o is dissolved in deionized water, under 70 DEG C of conditions, stir 1h;
(2) again by 2 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 2mol/L, until stop when pH is 11 dripping, then reacts 2h; Reaction terminates rear washed with de-ionized water throw out 5 times, leaves standstill 12h, then is poured out by supernatant liquor, continues to use washed with de-ionized water 3 times, then uses washes of absolute alcohol 3 times, under 40 DEG C of conditions, carry out vacuum drying, grinding, cross 200 mesh sieve, obtain Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 4 (mass ratio) with water, under 85 DEG C of conditions, stir 4h, obtains organo-mineral complexing magnetic and carries suspension agent.
Embodiment 2:
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Claim the Na-MMT of 100 parts, 3h is dried under 120 DEG C of conditions, cross 300 mesh sieve, add in reactor, then add the hydrochloric acid soln of the 2mol/L that 50 parts prepare, mechanical stirring 4h under 25 DEG C of conditions, leave standstill 36h, again supernatant liquor is poured out, be suspended thing 10 times by washed with de-ionized water, then by Na-MMT centrifugal 40min on the whizzer of 10000rpm.After end, throw out is dried under 120 DEG C of conditions, grinding, crosses 300 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 100: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 2.5h, mechanical stirring 3h under 80 DEG C of conditions; Then slowly add PEG4000 according to Na-MMT: PEG mass ratio 1: 0.4, stirring velocity is promoted to 1500rpm, continues reaction 4h, under 80 DEG C of conditions, carry out vacuum-drying 24h, grinding, cross 300 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 100 parts and 6000 parts of deionized waters, then add 130 parts of FeCl 36H 2o is dissolved in deionized water, under 80 DEG C of conditions, stir 2h;
(2) again by 80 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 4mol/L, until stop when pH is 11 dripping, then reacts 5h.Reaction terminates rear washed with de-ionized water throw out 7 times, leaves standstill 24h, then is poured out by supernatant liquor, continues to use washed with de-ionized water 4 times, then uses washes of absolute alcohol 4 times, under 80 DEG C of conditions, carry out vacuum drying, grinding, cross 300 mesh sieve, obtain Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 12 (mass ratio) with water, under 90 DEG C of conditions, stir 6h, obtains organo-mineral complexing magnetic and carries suspension agent.
Embodiment 3:
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Take the Na-MMT of 75 parts, under 110 DEG C of conditions, dry 2.5h, cross 250 mesh sieve, add in reactor, then add the hydrochloric acid soln of the 1.25mol/L that 30 parts prepare, mechanical stirring 3h under 25 DEG C of conditions, leave standstill 30h, then supernatant liquor is poured out, be suspended thing 8 times by washed with de-ionized water, again by Na-MMT centrifugal 35min on the whizzer of 6500rpm, after end, throw out is dried under 110 DEG C of conditions, grinding, cross 250 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 75: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 1.5h, mechanical stirring 2h under 65 DEG C of conditions.Then slowly add PEG3000 according to Na-MMT: PEG mass ratio 1: 0.22, stirring velocity is promoted to 1250rpm, continues reaction 3h, under 60 DEG C of conditions, carry out vacuum-drying 10h, grinding, cross 250 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 75 parts and 4000 parts of deionized waters, then add 70 parts of FeCl 36H 2o is dissolved in deionized water, under 75 DEG C of conditions, stir 1.5h;
(2) again by 41 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 3mol/L, until stop when pH is 11 dripping, then reacts 3.5h.Reaction terminates rear washed with de-ionized water throw out 6 times, leaves standstill 18h, then is poured out by supernatant liquor, continues to use washed with de-ionized water 3 times, then uses washes of absolute alcohol 3 times, under 60 DEG C of conditions, carry out vacuum drying, grinding, cross 250 mesh sieve, obtain Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 8 (mass ratio) with water, under 87 DEG C of conditions, stir 5h, obtains organo-mineral complexing magnetic and carries suspension agent.
Embodiment 4:
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Take the Na-MMT of 60 parts, 2h is dried under 104 DEG C of conditions, cross 200 mesh sieve, add in reactor, then add the hydrochloric acid soln of the 0.75mol/L that 18 parts prepare, mechanical stirring 2h under 25 DEG C of conditions, leave standstill 26h, again supernatant liquor is poured out, be suspended thing 7 times by washed with de-ionized water, then by Na-MMT centrifugal 32min on the whizzer of 4000rpm.After end, throw out is dried under 104 DEG C of conditions, grinding, crosses 200 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 60: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 0.5h, mechanical stirring 1.5h under 55 DEG C of conditions.Then slowly add PEG2000 according to Na-MMT: PEG mass ratio 1: 0.1, stirring velocity is promoted to 1100rpm, continues reaction 2.5h, under 45 DEG C of conditions, carry out vacuum-drying 8h, grinding, cross 200 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 60 parts and 2600 parts of deionized waters, then add 30 parts of FeCl 36H 2o is dissolved in deionized water, under 72 DEG C of conditions, stir 1h;
(2) again by 20 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 2.4mol/L, until stop when pH is 11 dripping, then reacts 2.5h.Reaction terminates rear washed with de-ionized water throw out 5 times, leaves standstill 14h, then is poured out by supernatant liquor, continues to use washed with de-ionized water 3 times, then uses washes of absolute alcohol 3 times, under 48 DEG C of conditions, carry out vacuum drying, grinding, cross 200 mesh sieve, obtain Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 4.5 (mass ratio) with water, under 86 DEG C of conditions, stir 4h, obtains organo-mineral complexing magnetic and carries suspension agent.
Embodiment 5:
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Take the Na-MMT of 70 parts, 2.5h is dried under 108 DEG C of conditions, cross 250 mesh sieve, add in reactor, then add the hydrochloric acid soln of the 1mol/L that 26 parts prepare, mechanical stirring 2.5h under 25 DEG C of conditions, leave standstill 28h, again supernatant liquor is poured out, be suspended thing 8 times by washed with de-ionized water, then by Na-MMT centrifugal 34min on the whizzer of 5000rpm.After end, throw out is dried under 108 DEG C of conditions, grinding, crosses 250 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 70: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 1h, mechanical stirring 2h under 60 DEG C of conditions.Then slowly add PEG3000 according to Na-MMT: PEG mass ratio 1: 0.15, stirring velocity is promoted to 1200rpm, continues reaction 3h, under 50 DEG C of conditions, carry out vacuum-drying 11h, grinding, cross 250 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 70 parts and 3200 parts of deionized waters, then add 50 parts of FeCl 36H 2o is dissolved in deionized water, under 74 DEG C of conditions, stir 1.5h;
(2) again by 30 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 2.8mol/L, until stop when pH is 11 dripping, then reacts 3h.Reaction terminates rear washed with de-ionized water throw out 6 times, leaves standstill 16h, then is poured out by supernatant liquor, continues to use washed with de-ionized water 4 times, then uses washes of absolute alcohol 4 times, under 50 DEG C of conditions, carry out vacuum drying, grinding, cross 250 mesh sieve, obtain Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 6 (mass ratio) with water, under 87 DEG C of conditions, stir 4.5h, obtains organo-mineral complexing magnetic and carries suspension agent.
Embodiment 6:
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Take the Na-MMT of 80 parts, 3h is dried under 112 DEG C of conditions, cross 300 mesh sieve, add in reactor, then add the hydrochloric acid soln of the 1.25mol/L that 34 parts prepare, mechanical stirring 3h under 25 DEG C of conditions, leave standstill 30h, again supernatant liquor is poured out, be suspended thing 9 times by washed with de-ionized water, then by Na-MMT centrifugal 36min on the whizzer of 6000rpm.After end, throw out is dried under 112 DEG C of conditions, grinding, crosses 300 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 80: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 1.5h, mechanical stirring 2.5h under 65 DEG C of conditions.Then slowly add PEG4000 according to Na-MMT: PEG mass ratio 1: 0.2, stirring velocity is promoted to 1300rpm, continues reaction 3.5h, under 55 DEG C of conditions, carry out vacuum-drying 14h, grinding, cross 300 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 80 parts and 3800 parts of deionized waters, then add 70 parts of FeCl 36H 2o is dissolved in deionized water, under 76 DEG C of conditions, stir 1.5h;
(2) again by 50 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 3.2mol/L, until stop when pH is 11 dripping, then reacts 3.5h.Reaction terminates rear washed with de-ionized water throw out 6 times, leaves standstill 18h, then is poured out by supernatant liquor, continues to use washed with de-ionized water 3 times, then uses washes of absolute alcohol 4 times, under 55 DEG C of conditions, carry out vacuum drying, grinding, cross 300 mesh sieve, obtain Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 7.5 (mass ratio) with water, under 87 DEG C of conditions, stir 5h, obtains organo-mineral complexing magnetic and carries suspension agent.
Embodiment 7:
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Take the Na-MMT of 90 parts, 2.5h is dried under 116 DEG C of conditions, cross 250 mesh sieve, add in reactor, then add the hydrochloric acid soln of the 1.5mol/L that 42 parts prepare, mechanical stirring 3.5h under 25 DEG C of conditions, leave standstill 32h, again supernatant liquor is poured out, be suspended thing 8 times by washed with de-ionized water, then by Na-MMT centrifugal 38min on the whizzer of 7000rpm.After end, throw out is dried under 116 DEG C of conditions, grinding, crosses 250 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 90: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 1h, mechanical stirring 2h under 70 DEG C of conditions.Then slowly add PEG3000 according to Na-MMT: PEG mass ratio 1: 0.25, stirring velocity is promoted to 1400rpm, continues reaction 3h, under 65 DEG C of conditions, carry out vacuum-drying 17h, grinding, cross 250 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 90 parts and 4400 parts of deionized waters, then add 90 parts of FeCl 36H 2o is dissolved in deionized water, under 77 DEG C of conditions, stir 1h;
(2) again by 60 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 3.6mol/L, until stop when pH is 11 dripping, then reacts 4h.Reaction terminates rear washed with de-ionized water throw out 6 times, leaves standstill 20h, then is poured out by supernatant liquor, continues to use washed with de-ionized water 4 times, then uses washes of absolute alcohol 3 times, under 60 DEG C of conditions, carry out vacuum drying, grinding, cross 250 mesh sieve, obtain Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 9 (mass ratio) with water, under 88 DEG C of conditions, stir 5.5h, obtains organo-mineral complexing magnetic and carries suspension agent.
Embodiment 8:
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Take the Na-MMT of 85 parts, 2.5h is dried under 114 DEG C of conditions, cross 300 mesh sieve, add in reactor, then add the hydrochloric acid soln of the 1.75mol/L that 40 parts prepare, mechanical stirring 3h under 25 DEG C of conditions, leave standstill 34h, again supernatant liquor is poured out, be suspended thing 9 times by washed with de-ionized water, then by Na-MMT centrifugal 37min on the whizzer of 8000rpm.After end, throw out is dried under 117 DEG C of conditions, grinding, crosses 250 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 85: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 1.5h, mechanical stirring 2.5h under 75 DEG C of conditions.Then slowly add PEG2000 according to Na-MMT: PEG mass ratio 1: 0.3, stirring velocity is promoted to 1350rpm, continues reaction 3.5h, under 70 DEG C of conditions, carry out vacuum-drying 20h, grinding, cross 200 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 85 parts and 5000 parts of deionized waters, then add 110 parts of FeCl 36H 2o is dissolved in deionized water, under 78 DEG C of conditions, stir 1.5h;
(2) again by 70 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 3.5mol/L, until stop when pH is 11 dripping, then reacts 4.5h.Reaction terminates rear washed with de-ionized water throw out 7 times, leaves standstill 22h, then is poured out by supernatant liquor, continues to use washed with de-ionized water 3 times, then uses washes of absolute alcohol 3 times, under 70 DEG C of conditions, carry out vacuum drying, grinding, cross 200 mesh sieve, obtain Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 10 (mass ratio) with water, under 89 DEG C of conditions, stir 5.5h, obtains organo-mineral complexing magnetic and carries suspension agent.
Embodiment 9:
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Take the Na-MMT of 95 parts, 2.5h is dried under 115 DEG C of conditions, cross 300 mesh sieve, add in reactor, then add the hydrochloric acid soln of the 1.8mol/L that 46 parts prepare, mechanical stirring 3.5h under 25 DEG C of conditions, leave standstill 34h, again supernatant liquor is poured out, be suspended thing 8 times by washed with de-ionized water, then by Na-MMT centrifugal 38min on the whizzer of 9000rpm.After end, throw out is dried under 119 DEG C of conditions, grinding, crosses 300 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 95: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 2h, mechanical stirring 3h under 77 DEG C of conditions.Then slowly add PEG3000 according to Na-MMT: PEG mass ratio 1: 0.35, stirring velocity is promoted to 1450rpm, continues reaction 3.5h, under 75 DEG C of conditions, carry out vacuum-drying 22h, grinding, cross 250 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 95 parts and 5500 parts of deionized waters, then add 120 parts of FeCl 36H 2o is dissolved in deionized water, under 79 DEG C of conditions, stir 2h;
(2) again by 75 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 3.7mol/L, until stop when pH is 11 dripping, then reacts 4h.Reaction terminates rear washed with de-ionized water throw out 6 times, leaves standstill 24h, then is poured out by supernatant liquor, continues to use washed with de-ionized water 4 times, then uses washes of absolute alcohol 4 times, under 75 DEG C of conditions, carry out vacuum drying, grinding, cross 250 mesh sieve, obtain Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 11 (mass ratio) with water, under 90 DEG C of conditions, stir 5.5h, obtains organo-mineral complexing magnetic and carries suspension agent.
Embodiment 10:
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Take the Na-MMT of 85 parts, 3h is dried under 110 DEG C of conditions, cross 250 mesh sieve, add in reactor, then add the hydrochloric acid soln of the 1.8mol/L that 48 parts prepare, mechanical stirring 4h under 25 DEG C of conditions, leave standstill 36h, again supernatant liquor is poured out, be suspended thing 7 times by washed with de-ionized water, then by Na-MMT centrifugal 35min on the whizzer of 8500rpm.After end, throw out is dried under 115 DEG C of conditions, grinding, crosses 300 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 85: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 2.5h, mechanical stirring 3h under 79 DEG C of conditions.Then slowly add PEG4000 according to Na-MMT: PEG mass ratio 1: 0.4, stirring velocity is promoted to 1500rpm, continues reaction 4h, under 77 DEG C of conditions, carry out vacuum-drying 20h, grinding, cross 250 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 85 parts and 5300 parts of deionized waters, then add 115 parts of FeCl 36H 2o is dissolved in deionized water, under 77 DEG C of conditions, stir 2h;
(2) again by 70 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 3.5mol/L, until stop when pH is 11 dripping, then reacts 4.5h.Reaction terminates rear washed with de-ionized water throw out 5 times, leaves standstill 24h, then is poured out by supernatant liquor, continues to use washed with de-ionized water 4 times, then uses washes of absolute alcohol 3 times, under 77 DEG C of conditions, carry out vacuum drying, grinding, cross 300 mesh sieve, obtain Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 10.5 (mass ratio) with water, under 87 DEG C of conditions, stir 6h, obtains organo-mineral complexing magnetic and carries suspension agent.

Claims (1)

1. organo-mineral complexing magnetic carries a production method for suspension agent, it is characterized in that: produced by following steps, (the thing amount " part " of getting is weight part)
The first step: the acidification of sodium-based montmorillonite (Na-MMT)
Take the Na-MMT of 50 ~ 100 parts, 2 ~ 3h is dried under 100 ~ 120 DEG C of conditions, cross 200 ~ 300 mesh sieve, add in reactor, then add the hydrochloric acid soln of 0.5 ~ 2mol/L that 10 ~ 50 parts prepare, mechanical stirring 2 ~ 4h under 25 DEG C of conditions, leave standstill 24 ~ 36h, again supernatant liquor is poured out, be suspended thing 6 ~ 10 times by washed with de-ionized water, then by Na-MMT centrifugal 30 ~ 40min on the whizzer of 3000 ~ 10000rpm; After end, throw out is dried under 100 ~ 120 DEG C of conditions, grinding, crosses 200 ~ 300 mesh sieve, for subsequent use;
Second step: the preparation of polyoxyethylene glycol (PEG) solution intercalation Na-MMT
According to dehydrated alcohol: Na-MMT mass ratio 50 ~ 100: 1, the Na-MMT after acidifying is joined in reactor, ultrasonic 0.5 ~ 2.5h, mechanical stirring 1 ~ 3h under 50 ~ 80 DEG C of conditions; Then slowly PEG2000 ~ 4000 are added according to Na-MMT: PEG mass ratio 1: 0.05 ~ 0.4, stirring velocity is promoted to 1000 ~ 1500rpm, continue reaction 2 ~ 4h, vacuum-drying 5 ~ 24h is carried out under 40 ~ 80 DEG C of conditions, grinding, cross 200 ~ 300 mesh sieve, obtain organobentonite (OMMT), for subsequent use;
3rd step: Fe 3o 4load OMMT prepares organo-mineral complexing magnetic and carries suspension agent
(1) N is being connected with 2seal pot in, add OMMT 50 ~ 100 parts and 2000 ~ 6000 parts of deionized waters, then add 10 ~ 130 parts of FeCl 36H 2o is dissolved in deionized water, under 70 ~ 80 DEG C of conditions, stir 1 ~ 2h;
(2) again by 2 ~ 80 parts of FeCl 24H 2o slowly joins in reactor, and then dropwise drips the NaOH solution of 2 ~ 4mol/L, until stop when pH is 11 dripping, then reacts 2 ~ 5h; Reaction terminates rear washed with de-ionized water throw out 5 ~ 7 times, leaves standstill 12 ~ 24h, then is poured out by supernatant liquor, continue to use washed with de-ionized water 3 ~ 4 times, then use washes of absolute alcohol 3 ~ 4 times, under 40 ~ 80 DEG C of conditions, carry out vacuum drying, grinding, crosses 200 ~ 300 mesh sieve, obtains Fe 3o 4load OMMT, for subsequent use;
(3) dry Fe is got 3o 4load OMMT mixes with 1: 4 ~ 12 (mass ratioes) with water, stirs 4 ~ 6h, obtain organo-mineral complexing magnetic and carry suspension agent under 85 ~ 90 DEG C of conditions.
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