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A diblock macromolecular quaternary ammonium salt containing polysiloxane chain segment and its preparation method and application

A technology of polysiloxane and polydimethylsiloxane, which is applied in the field of diblock macromolecular quaternary ammonium salt and its preparation, can solve the problems of loss, insufficient adsorption and the like, achieve no by-products, and optimize the purification work. , the effect of improving productivity

Active Publication Date: 2020-12-22
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, small-molecule pesticides are easily lost with irrigation water due to insufficient adsorption, resulting in the need for large doses of spraying to make up for their lack of efficiency

Method used

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  • A diblock macromolecular quaternary ammonium salt containing polysiloxane chain segment and its preparation method and application
  • A diblock macromolecular quaternary ammonium salt containing polysiloxane chain segment and its preparation method and application
  • A diblock macromolecular quaternary ammonium salt containing polysiloxane chain segment and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Preparation of diblock macromolecular quaternary ammonium salt containing polysiloxane segment:

[0062] The ratio of the degree of polymerization of the polysiloxane block segment to the quaternized polydimethylaminoethyl methacrylate segment is PDMS:QPDMAEMA=27:18, the length of the PDMS block is 2kDa, and the length of the QPDMAEMA block is 5kDa. The preparation process is as figure 1 As shown, the specific steps are as follows:

[0063] (1) In a Schlenk bottle equipped with a magnetic stirring bar, add 50g D 3 , and then seal it with a silica gel stopper, vacuumize the inside of the bottle and feed high-purity nitrogen, repeat the operation three times to ensure that the bottle is filled with nitrogen. Inject 100mL of dry tetrahydrofuran into a syringe to dissolve D 3 After obtaining a clear solution, inject 10 mL of n-hexane solution containing 2.5 mol / L n-butyllithium at 0°C to initiate anionic ring-opening polymerization. After keeping stirring at 0°C for abo...

Embodiment 2

[0069] Preparation of diblock macromolecular quaternary ammonium salt containing polysiloxane segment:

[0070] The polymerization degree ratio of the polysiloxane block segment and the quaternized polydimethylaminoethyl methacrylate segment is PDMS:QPDMAEMA=40:18, the length of the PDMS block is 3kDa, and the length of the QPDMAEMA block is 5kDa. The preparation process is as figure 1 As shown, the steps of Example 1 are roughly the same, the only difference being:

[0071] The injection volume of n-butyllithium in step (1) is 6.67mL, the time to keep stirring at 0°C is about 18h, and the feed volume of dimethylvinylchlorosilane is 2.01g;

[0072] In step (2), the charging capacity of mercaptoethanol is 1.04g;

[0073] In step (3), the charging capacity of triethylamine and 2-bromoisobutyryl bromide is respectively 1.01g and 2.30g;

[0074] The charging capacity of PDMS-Br is 10.83g in the step (4);

[0075] The charging capacity of benzyl chloride is 3.87g in the step (5...

Embodiment 3

[0078] Preparation of diblock macromolecular quaternary ammonium salt containing polysiloxane segment:

[0079] The ratio of the degree of polymerization of the polysiloxane block segment to the quaternized polydimethylaminoethyl methacrylate segment is PDMS:QPDMAEMA=54:18, the length of the PDMS block is 4kDa, and the length of the QPDMAEMA block is 5kDa. The preparation process is as figure 1 As shown, the steps of Example 1 are roughly the same, the only difference being:

[0080] The injection volume of n-butyllithium in step (1) is 5.00mL, the time to keep stirring at 0°C is about 24h, and the feeding volume of dimethylvinylchlorosilane is 1.51g;

[0081] In step (2), the charging capacity of mercaptoethanol is 0.78g;

[0082] In step (3), the charging capacity of triethylamine and 2-bromoisobutyryl bromide is respectively 0.76g and 1.73g;

[0083] The charging capacity of PDMS-Br is 14.44g in the step (4);

[0084] The charging capacity of benzyl chloride is 3.30g in...

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Abstract

The invention discloses a diblock macromolecular quaternary ammonium salt containing a polyorganosiloxane chain block and preparation method and application thereof. The preparation method comprises the steps that polyorganosiloxane of which a single end is a vinyl group is firstly synthesized; the polyorganosiloxane of which the single end is a hydroxyl group is synthesized through the click reaction with mercaptoethanol; reaction between the polyorganosiloxane with the single ended hydroxyl group and alpha-bromoisobutyryl bromide is conducted to synthesize a polyorganosiloxane macromolecularevocating agent, and DMAPMA is evocated to conduct the polymerization of ATRP; finally benzyl chloride is used for conducting quaternization to synthesize the diblock macromolecular quaternary ammonium salt containing the polyorganosiloxane chain block. According to the diblock macromolecular quaternary ammonium salt containing the polyorganosiloxane chain block, the macromolecular quaternary ammonium salt which has amphipathy has good absorbing and infiltrating capabilities on sclerotium of thanatephorus cucumeris, and therefore the macromolecular quaternary ammonium salt has good inhibitingeffect on the germination of the sclerotium.

Description

technical field [0001] The invention belongs to the field of synthesis and application of polymer materials, in particular to a two-block macromolecule quaternary ammonium salt containing polysiloxane chain segments and a preparation method and application thereof. Background technique [0002] Rice sheath blight, also known as "cloud pattern", commonly known as "flower foot stem", is widely distributed in major rice producing countries in the world, and has become the first of the three major diseases of rice in my country. Rice sheath blight is a soil-borne disease caused by Rhizoctonia solani (R.solani), which mainly reproduces asexually. There are two main forms of the fungus in the natural state, namely hyphae and sclerotia. An important reason for the serious damage of rice sheath blight lies in the infection cycle of "sclerotia germination to form hyphae-mycelia infecting the host-mycelium aggregates to form sclerotia under forced conditions". [0003] The current p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/452A01P3/00
CPCC08G77/452
Inventor 张安强钟伟强林雅铃董辰韵常瑶瑶
Owner SOUTH CHINA UNIV OF TECH
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