CN112341487A

CN112341487A - Hyperbranched polysiloxane blocking agent and preparation method thereof

Info

Publication number: CN112341487A
Application number: CN202011081562.5A
Authority: CN
Inventors: 袁明进; 罗霄; 胡进科; 朱智超; 卢福伟
Original assignee: China Petroleum and Chemical Corp; Sinopec East China Co
Current assignee: China Petroleum and Chemical Corp; Sinopec East China Co
Priority date: 2020-10-12
Filing date: 2020-10-12
Publication date: 2021-02-09
Anticipated expiration: 2040-10-12
Also published as: CN112341487B

Abstract

The invention discloses a hyperbranched polysiloxane blocking agent and a preparation method thereof, wherein erythritol is used as a raw material, and an oxidation reaction, an amination reaction and a Michael addition reaction are sequentially carried out on the erythritol in a solution to obtain a final product

The method has the advantages of simple process, low cost, mild conditions, good safety and high yield, and is suitable for industrial production; the prepared hyperbranched polysiloxane blocking agent has the characteristics of precise and controllable molecular size and structure, siloxane groups contained in end groups and high group density, can be quickly gelled and deposited to form a compact blocking layer after entering a reservoir seepage channel, effectively blocks drilling fluid filtrate from invading the seepage channel, and further greatly improves the wellThe wall stability is high, and the water-based drilling fluid prepared by taking the water-based drilling fluid as a key auxiliary agent can effectively inhibit the hydration expansion and dispersion of bentonite and improve the rolling recovery rate of the shale.

Description

Hyperbranched polysiloxane blocking agent and preparation method thereof

Technical Field

The invention relates to a hyperbranched polysiloxane blocking agent for blocking a micro seepage channel of a reservoir in an oil drilling process and a preparation method thereof.

Background

When the water-based drilling fluid is used for drilling a shale gas reservoir, the drilling fluid filtrate is very easy to invade a seepage channel of the reservoir under the action of differential pressure, so that the phenomena of hydration expansion of clay minerals, dislocation slippage of a rock cementing surface, hydraulic wedge of cracks and the like in the reservoir are caused, the borehole wall is reduced in diameter and falls into blocks, and unfavorable well conditions such as drill bit balling, drilling tool jamming and the like are caused.

Under the action of high temperature in a well, siloxane groups can be hydrolyzed in water-based drilling fluid with the pH value of 11-12, water-soluble micromolecules containing the siloxane groups form polymers with negative charges, the polymerization degree of the polymers is usually very low due to the mutual repulsion of the negative charges, the fluid radius of the oligomers is very small, the oligomers can enter tiny pores of a shale reservoir layer along with filtrate, the pH value of the pore fluid is close to neutral, the repulsion force among the oligomers is greatly reduced along with the filtrate after the filtrate is diluted by the fluid, and then etherification and glue formation are carried out to form a three-dimensional silicone gel network to block seepage channels. While the pore fluid contains Ca in large amount²⁺、Mg²⁺When the polyvalent cation and oligomer are contacted with the polyvalent cation and oligomer, water-insoluble silicate precipitate can be quickly formed. The gel and the precipitate quickly form a compact plugging layer, so that the pore pressure transmission and the further invasion of filtrate can be blocked in a very short time, and the well wall can be sealed. In addition, the silicate drilling fluid formed on the basis of the organic silicon can greatly reduce the water activity, and is favorable for blocking water from a well hole to the wall of the wellThe migration of the rock further stabilizes the borehole wall.

However, although the existing conventional polymer can form a compact blocking layer and block the migration of water from a well bore to a wall rock of the well bore so as to stabilize the well bore, the preparation process is complex, the preparation cost is high, the yield is low, in addition, the molecular size and the structure are not controllable, and the formation time of the compact blocking layer is long after the polymer is mixed with filtrate reservoir pore fluid.

Disclosure of Invention

The invention aims to solve the technical problem of providing a hyperbranched polysiloxane blocking agent which has simple process, low cost, mild conditions, good safety, high yield, precise and controllable molecular size and structure, primary amine group as a terminal group and high group density, thereby forming a compact blocking layer formed by gel and precipitation together in a short time and rapidly blocking filtrate permeation and pore pressure transmission, and a preparation method thereof.

In order to solve the technical problems, the hyperbranched polysiloxane-based plugging agent is prepared by taking erythritol as a raw material and sequentially carrying out oxidation reaction, amination reaction and Michael addition reaction, and has the following structural formula:

the preparation method of the hyperbranched polysiloxane plugging agent comprises the following steps:

(1) adding chromium trioxide into hydrochloric acid while stirring, mixing to obtain a solution A, cooling the solution A to 0 ℃, dropwise adding pyridine into the solution A within 10min, keeping the temperature at 0 ℃ for reacting for 2-4 h to obtain a PCC crude product, and drying the PCC crude product to obtain a pure PCC reagent;

(2) completely dissolving a PCC reagent in an organic solvent a to obtain a solution B, and dropwise adding a solution C into the solution B under the condition of stirring at room temperature, wherein the solution C is obtained by completely dissolving erythritol in the organic solvent a; reacting for 3-6 h after the dropwise adding is finished to obtain a mixed solution of 2, 3-dioxo-butanedialdehyde, and purifying to obtain the 2, 3-dioxo-butanedialdehyde;

(3) pouring ammonium formate and formic acid into an excessive organic solvent b, and stirring to obtain a solution D; heating the solution D to 60-90 ℃, and adding a solution E into the solution D, wherein the solution E is obtained by completely dissolving 2, 3-dioxosuccinaldehyde in an organic solvent b; after the dropwise addition, heating to 140-160 ℃ for reaction for 4-8 h to obtain a mixed solution of 1,2,3, 4-tetraaminobutane, and purifying to obtain 1,2,3, 4-tetraaminobutane;

(4) pouring 1,2,3, 4-tetraaminobutane into an excessive organic solvent c, and stirring to obtain a solution F; heating the solution to 50-60 ℃, and adding a solution G into the solution F, wherein the solution G is obtained by completely dissolving gamma-methacryloxypropyltrimethoxysilane in an organic solvent c; continuously reacting for 5-10 h at 50-70 ℃ after the dripping is finished to obtain mixed liquid of the hyperbranched polysiloxane-based plugging agent, and purifying to obtain the final product of the hyperbranched polysiloxane-based plugging agent

In the step (1), the concentration of the hydrochloric acid is 5-8 mol/L.

In the step (1), the molar ratio of HCl to chromium trioxide in hydrochloric acid is 1 (1-2).

In the step (1), the molar ratio of the chromium trioxide to the pyridine is 1:1.

In the step (2), the molar ratio of hydroxyl of erythritol to the PCC reagent is 1 (1.3-1.5).

In the step (2), the organic solvent a is dichloromethane, trichloromethane or tetrahydrofuran after water removal.

In the step (3), the molar ratio of ammonium formate to formic acid is 1 (2-3), and the total molar amount of ammonium formate and formic acid is 2-4 times of 2, 3-dioxosuccinaldehyde.

In the step (3), the organic solvent b is toluene, tetrahydrofuran or N, N-dimethyl formamide.

In the step (4), the organic solvent c is dimethyl sulfoxide, tetrahydrofuran or N, N-dimethyl formamide.

In the step (4), the molar ratio of 1,2,3, 4-tetraaminobutane to gamma-methacryloxypropyltrimethoxysilane is 1 (8-12).

The invention has the following characteristics and beneficial effects:

(1) the invention takes the erythritol as the raw material, and the erythritol is sequentially subjected to oxidation reaction, amination reaction and Michael addition reaction in the solution, so as to obtain the final product.

(2) The hyperbranched polysiloxane blocking agent prepared by the invention has the characteristics of precise and controllable molecular size and structure, primary amine group as a terminal group and high group density, and can form a compact blocking layer formed by gel and precipitation in a very short time after the blocking agent is mixed with pore fluid of a filtrate storage layer, thereby rapidly blocking the filtrate permeation and the pore pressure transmission.

(3) The method is characterized in that proper hyperbranched micromolecules are selected, the end groups of the hyperbranched micromolecules are correspondingly modified, the hyperbranched polysiloxane blocking agent with siloxane groups as end groups is obtained, different from linear molecules, the end groups of the hyperbranched micromolecules are positioned on a plurality of branch arms of the molecules, high-density end groups can be integrated on limited molecular sizes, the siloxane groups on the end groups of the molecules can be hydrolyzed underground to form silicon hydroxyl groups, then oligomers with small sizes are formed, and after the oligomers enter a reservoir seepage channel along with filtrate, the oligomers are rapidly crosslinked to form gel or precipitate, so that the filtrate seepage and pore pressure transmission are effectively blocked.

(4) Because the terminal group density of the hyperbranched micromolecules is extremely high, oligomers formed by the molecules have a plurality of etherification gel forming points and salifying bonding points of the etherification gel forming points and the salifying bonding points with metal cations, so that a compact blocking layer can be formed in a very short time.

(5) The steric hindrance effect between the branched arms ensures that the silicon hydroxyl groups at the end parts of the branched arms are distributed in a spatially divergent manner, which is beneficial to the combination of oligomers to form gel, increases the trapping probability of the oligomers on metal cations and is also beneficial to the rapid formation of a blocking layer.

Drawings

FIG. 1 is an infrared spectrum obtained in example 4;

FIG. 2 is a schematic view of an embodimentExample 4 obtained¹HNMR map.

Detailed Description

The present invention will be further described with reference to the following specific examples, wherein the following percentages are by mass unless otherwise specified.

Example 1

This example is a preparation example of a PCC reagent, and it should be noted that, in the chemical field, a PCC reagent is a complex salt solution of chromium trioxide and pyridine in hydrochloric acid.

Adding chromium trioxide into hydrochloric acid while stirring, mixing to obtain a solution A, cooling the solution A to 0 ℃, dropwise adding pyridine into the solution A within 10min, keeping the temperature at 0 ℃ for reacting for 2-4 h to obtain a PCC crude product, and drying the PCC crude product to obtain a pure PCC reagent, wherein the specific preparation method of the embodiment is as follows:

quickly adding 100g of chromium trioxide (the molar ratio of HCl to chromium trioxide in hydrochloric acid is 1 (1-2)) into 184mL of hydrochloric acid (the concentration of HCl is 5-8 mol/L (preferably 6 mol/L)) with stirring, cooling the homogeneous solution to 0 ℃ after 5min to obtain a reddish brown liquid, and filtering at normal pressure to remove insoluble substances; then, within 10min, adding 79.1g of pyridine into the homogeneous solution, gradually precipitating yellow solid along with the addition of the pyridine, dropwise adding the pyridine (the molar ratio of chromium trioxide to pyridine is 1:1), cooling to 0 ℃ again, reacting for 2-4 h (preferably 3h) to obtain orange solid, and filtering by using a sand core funnel to collect an orange solid product, namely a PCC crude product; the product was dried in a vacuum desiccator for 1h and then dried in a desiccator containing phosphorus pentoxide at ambient temperature for 48h to give 180g of the final product, i.e. pure PCC reagent, at 84% yield.

The involved reaction formula is as follows:

example 2

This example is a preparation of 2, 3-dioxosuccinaldehyde.

Completely dissolving a PCC reagent in an organic solvent a (the organic solvent a is dewatered dichloromethane, trichloromethane or tetrahydrofuran) to obtain a solution B, and dropwise adding a solution C into the solution B under the condition of stirring at room temperature, wherein the solution C is obtained by completely dissolving erythritol in the organic solvent a; after the dropwise addition, reacting for 3-6 h to obtain a mixed solution of 2, 3-dioxosuccinaldehyde, and purifying to obtain 2, 3-dioxosuccinaldehyde, wherein the specific method of the embodiment is as follows:

dichloromethane (DCM) was passed over anhydrous CaCl₂Drying, redistilling, dissolving the PCC reagent in DCM with water being redistilled, stirring, and pouring into a 500mL three-mouth flask after the PCC reagent is completely dissolved. Dropwise adding a DCM solution of erythritol into a three-neck flask under the condition of stirring at room temperature, ensuring that the molar ratio of hydroxyl of erythritol to a PCC reagent is 1 (1.3-1.5), preferably 1:1.5, and stopping reaction after continuously reacting for 4h after the dropwise adding is finished. Pouring out the upper layer solution, washing the lower layer solid substance with DCM for 3 times, combining the upper layer solution and the washing solution, and combining the combined solution with saturated NaHCO sequentially₃The resulting solution was washed with an aqueous solution, dried over anhydrous Na2SO4, filtered to remove the solvent, and the residue was distilled under reduced pressure to obtain a pale yellow crystal, i.e., 2, 3-dioxosuccinaldehyde.

The involved reaction formula is as follows:

it should be noted that all the DCM used in this example are the DCM after water re-evaporation.

Example 3

This example is a preparation example of 1,2,3, 4-tetraaminobutane.

Pouring ammonium formate and formic acid (the molar ratio of the ammonium formate to the formic acid is 1 (2-3), and the total molar amount of the ammonium formate and the formic acid is 2-4 times of 2, 3-dioxobutanedialdehyde) into an excessive organic solvent b (the organic solvent b is toluene, tetrahydrofuran or N, N-dimethylformamide), and stirring to obtain a solution D; heating the solution D to 60-90 ℃, and adding the solution E into the solution D, wherein the solution E is obtained by completely dissolving 2, 3-dioxosuccinaldehyde in an organic solvent b; after the dropwise addition, heating to 140-160 ℃ for reaction for 4-8 h to obtain a mixed solution of 1,2,3, 4-tetraaminobutane, and purifying to obtain 1,2,3, 4-tetraaminobutane, wherein the specific method of the embodiment is as follows:

weighing ammonium formate and formic acid according to a molar ratio of 1:2, uniformly stirring, pouring into excessive toluene, uniformly stirring again, and pouring into a three-neck flask with a condensing reflux pipe; heating to 80 ℃ under the condition of oil bath, and dropwise adding a toluene solution of 2, 3-dioxosuccinaldehyde into the three-neck flask; after the dropwise addition is finished, slowly heating the reaction solution system to 160 ℃, continuing to react for 6 hours, stopping the reaction to obtain black tar-like liquid, performing reduced pressure suction filtration to remove black coke impurities, and sequentially using saturated NaHCO for the obtained filtrate₃Washing with saturated NaCl aqueous solution, separating the separated liquid with separating funnel, and adding anhydrous Na₂SO₄Drying the mother liquor, and distilling the residual liquid under reduced pressure to obtain

white needle crystal

1,2,3, 4-tetraaminobutane (TABT). When erythritol, which is a raw material, is used as an evaluation standard, the yield of 1,2,3, 4-tetraaminobutane is 83.41%.

The reaction route is as follows:

after the 1,2,3, 4-tetraaminobutane is successfully prepared, it may be abbreviated as TABT according to its

English name

1,2,3, 4-tetraaminobutane, which is hereinafter referred to as TABT.

Example 4

This example is an example of the preparation of a hyperbranched polysiloxane-based blocking agent.

Pouring 1,2,3, 4-tetraaminobutane into an excessive organic solvent c (the organic solvent c is dimethyl sulfoxide, tetrahydrofuran or N, N-dimethylformamide), and stirring to obtain a solution F; heating the solution to 50-60 ℃, and adding a solution G into the solution F, wherein the solution G is obtained by completely dissolving gamma-methacryloxypropyltrimethoxysilane in an organic solvent c (the molar ratio of 1,2,3, 4-tetraaminobutane to gamma-methacryloxypropyltrimethoxysilane is 1 (8-12)); after the dropwise addition, the reaction is continued for 5 to 10 hours at the temperature of between 50 and 70 ℃ to obtain a mixed solution of the hyperbranched polysiloxane-based plugging agent, and the mixed solution is purified to obtain a final product of the hyperbranched polysiloxane-based plugging agent, wherein the specific preparation method of the embodiment is as follows:

pouring 1,2,3, 4-tetraaminobutane into excessive N, N-dimethylformamide, stirring uniformly, and pouring into a three-neck flask with a condensation reflux pipe. Heating to 60 ℃ under the condition of oil bath, and dropwise adding an N, N-dimethyl formamide solution of gamma-methacryloxypropyl trimethoxy silane into a three-neck flask; keeping the reaction temperature at 60 ℃ after the dropwise addition is finished, continuing the reaction for 9 hours, stopping the reaction to obtain light yellow oily liquid, performing reduced pressure suction filtration to remove black coke impurities, and sequentially using saturated NaHCO for the obtained filtrate₃Washing with saturated NaCl aqueous solution, separating the separated liquid with separating funnel, and adding anhydrous Na₂SO₄Drying the upper layer mother liquor, and finally carrying out reduced pressure distillation on the residual liquor to obtain a light yellow needle crystal, namely the hyperbranched polysiloxane-based blocking agent, wherein the product yield is 82.67%.

The reaction route is as follows:

wherein

FIG. 1 shows an infrared spectrum of the hyperbranched polysiloxane blocking agent, and the characteristic absorption peaks of the spectrum are analyzed as follows: 3453cm^-1The C ═ O bond stretching vibration absorption peak introduced by KH-57; 2927cm^-1Is treated as-CH in the product₂-a stretching vibration peak; 1724cm^-1Is treated as-N-CH in the product₃Absorption peak of (4); 1636cm^-1C ═ O bond bending vibration absorption peak introduced at KH-570; 1488cm^-1A characteristic absorption peak of Si-O introduced by KH-570; 1407cm^-1In the form of-O-CH introduced at KH-570₃Is bentA vibration absorption peak; 1096cm^-1The position is a C-N stretching vibration absorption peak in a molecular framework, and the molecular structure of the product is deduced to be consistent with the structure of a target product by knowing an infrared spectrogram of the product, wherein the molecular structure of the product has a pre-thought molecular group.

FIG. 2 shows a hyperbranched polysiloxane-based blocking agent¹HNMR picture, characteristic peak analysis of the map is as follows: delta 1.12 is-CH originally linked to an alpha, beta unsaturated carbon-carbon double bond₃The proton peak of (a); the proton peak of-NH-introduced by 1,2,3, 4-tetraaminobutane is at delta 1.52; delta 2.43 introduced by 1,2,3, 4-tetraaminobutane

A proton peak of (a); delta 2.87-CH introduced by gamma-methacryloxypropyltrimethoxysilane₂The proton peak at delta 3.39 is O-CH in the siloxy radical introduced by gamma-methacryloxypropyltrimethoxysilane₃The proton peak of (1). According to the infrared spectrogram, the structure of the test product is consistent with that of the target product, and the successful preparation of the required final product is indicated.

After the hyperbranched polysiloxane-based blocking agent has been successfully prepared, it may be referred to as HPBBA for short, and the product is hereinafter referred to as HPBBA.

Example 5

This example is an example of the formulation of HPBBA prepared in example 4 into a water-based drilling fluid.

Measuring 1000g of tap water, raising the temperature of the water to 65 ℃, adding 5g of KOH under electric stirring of 300r/min, stirring for 10min, adding 3g of HPBBA, stirring for 30min, increasing the stirring rate to 500r/min, adding 10g of polyanionic cellulose PAC-LV, stirring for 10min, adding 4g of viscosity-increasing and cutting agent JHVIS, stirring for 5min, adding 25g of filtrate reducer ShaleFLO, stirring for 5min, adding 15g of plugging and anti-collapse agent ShaleSeaL, stirring for 5min, adding 10g of nano plugging agent MicroSeaL, stirring for 5min, adding 10g of shale inhibitor UHIB, stirring for 5min, adding 6g of rheological aid JHX-RH, stirring for 5min, adding 5g of lubricant LUJHB, stirring for 10min, adding quantitative weight to adjust the density of the drilling fluid to a specified value, and continuing stirring for 2h to prepare the water-based drilling fluid system required for evaluation.

Example 6

This example is an example of the effect of the water-based drilling fluid prepared in example 5 on the slurrification performance of bentonite.

The capability of the water-based drilling fluid for inhibiting bentonite slurrying is evaluated according to a centrifugal method in a water injection clay stabilizer performance evaluation method of China's republic of China petroleum and gas industry standard SY/T5971-1994.

The method comprises the following specific steps:

weighing 0.50g of Xinjiang Xiazijie bentonite powder, accurately weighing the powder to 0.01g, filling the powder into a 10mL centrifugal tube, adding 10mL of water-based drilling fluid, fully shaking the mixture uniformly, storing the mixture for 2 hours at room temperature, filling the mixture into a centrifuge, and performing centrifugal separation for 15 minutes at the rotating speed of 2000 r/min. Reading out the volume V of the swelled bentonite₁；

② repeating the step I, replacing the inhibitor solution with 10mL of deionized water, and measuring the expansion volume V of the bentonite in the water₂；

Thirdly, repeating the step I, replacing the inhibitor solution with 10mL of kerosene, and measuring the volume V of the bentonite in the kerosene₀。

The anti-swelling rate calculation formula is as follows:

wherein: b-anti-swelling ratio, unit: percent; v₁-swell volume of bentonite in water-based drilling fluids, unit: mL; v₂-swell volume of bentonite in deionized water, unit: mL; v₀-swell volume of bentonite in kerosene, unit: and (mL).

The results are shown in Table 1.

TABLE 1 Effect of inhibitor dosage on anti-swelling Rate

System of	Percent swelling prevention (%)
		Water-based drilling fluid	92.6

As can be seen from the data in Table 1, the water-based drilling fluid using HPBBA as a key auxiliary agent can control the anti-swelling rate of bentonite to 92.6%, which shows that the drilling fluid can effectively inhibit the hydration slurrying of the bentonite.

Example 7

This example is an example of the effect of the water-based drilling fluid prepared in example 5 on mud shale slurrying performance.

The capability of the water-based drilling fluid for inhibiting drill chip dispersion slurrying is evaluated according to a shale dispersion test in a shale physical and chemical property test method of a petroleum and gas industry standard SY/T5613-2000 of the people's republic of China.

The method comprises the following specific steps:

taking outcrop of mud shale in the Sichuan Longmaxi stratum and drill cuttings, sieving the outcrop and the drill cuttings with a 6-10-mesh sieve, drying the outcrop and the drill cuttings to constant weight, weighing 50.0g of the outcrop and the drill cuttings, adding the outcrop and the drill cuttings into an aging tank containing 350mL of water-based drilling fluid, aging the mixture at 105 ℃ for 16 hours, taking out the aging tank, cooling the aging tank to room temperature, pouring liquid and the mud shale in the tank into a 40-mesh sorting sieve, and washing the mud shale with tap water for 1 min. Putting the separation sieve and the shale into a drying box, drying for 4h at (105 +/-3) ℃, taking out, cooling, standing in air for 24h, weighing and recording data M, and calculating the rolling recovery rate R.

The rolling recovery calculation formula is as follows:

wherein: r-drill cuttings recovery, unit: percent; m-drill cuttings recovery after hot rolling, unit: g.

the results are shown in Table 2.

TABLE 2 Effect of inhibitor dosage on Rolling recovery

As can be seen from the data in Table 2, the rolling recovery rates of outcrops and cuttings of the shale in the water-based drilling fluid both exceed 98%, which indicates that the water-based drilling fluid using HPBBA as a key auxiliary agent can effectively inhibit the hydration dispersion of the shale.

Claims

1. A hyperbranched polysiloxane blocking agent is characterized in that: the erythritol is used as a raw material and is prepared by oxidation reaction, amination reaction and Michael addition reaction in sequence, and the structural formula of the erythritol is as follows:

2. a preparation method of a hyperbranched polysiloxane blocking agent comprises the following steps:

(4) pouring 1,2,3, 4-tetraaminobutane into an excessive organic solvent c, and stirring to obtain a solution F; heating the solution to 50-60 ℃, and adding a solution G into the solution F, wherein the solution G is obtained by completely dissolving gamma-methacryloxypropyltrimethoxysilane in an organic solvent c; continuously reacting for 5 to 10 hours at the temperature of between 50 and 70 ℃ after the dropwise addition is finished to obtain mixed liquid of the hyperbranched polysiloxane blocking agent, and purifying to obtain the final product of the hyperbranched polysiloxane blocking agent

3. The process for the preparation of a hyperbranched polysiloxane-based blocking agent according to claim 2, wherein: in the step (1), the concentration of the hydrochloric acid is 5-8 mol/L.

4. The process for the preparation of a hyperbranched polysiloxane-based blocking agent according to claim 2, wherein: in the step (1), the molar ratio of HCl to chromium trioxide in hydrochloric acid is 1 (1-2).

5. The process for the preparation of a hyperbranched polysiloxane-based blocking agent according to claim 2, wherein: in the step (1), the molar ratio of the chromium trioxide to the pyridine is 1:1.

6. The process for the preparation of a hyperbranched polysiloxane-based blocking agent according to claim 2, wherein: in the step (2), the molar ratio of hydroxyl of erythritol to the PCC reagent is 1 (1.3-1.5).

7. The process for the preparation of a hyperbranched polysiloxane-based blocking agent according to claim 2, wherein: in the step (2), the organic solvent a is dichloromethane, trichloromethane or tetrahydrofuran after water removal.

8. The process for the preparation of a hyperbranched polysiloxane-based blocking agent according to claim 2, wherein: in the step (3), the molar ratio of ammonium formate to formic acid is 1 (2-3), and the total molar amount of ammonium formate and formic acid is 2-4 times of 2, 3-dioxosuccinaldehyde.

9. The process for the preparation of a hyperbranched polysiloxane-based blocking agent according to claim 2, wherein: in the step (3), the organic solvent b is toluene, tetrahydrofuran or N, N-dimethylformamide.

10. The process for the preparation of a hyperbranched polysiloxane-based blocking agent according to claim 2, wherein: in the step (4), the organic solvent c is dimethyl sulfoxide, tetrahydrofuran or N, N-dimethylformamide.

11. The process for the preparation of a hyperbranched polysiloxane-based blocking agent according to claim 2, wherein: in the step (4), the molar ratio of 1,2,3, 4-tetraaminobutane to gamma-methacryloxypropyltrimethoxysilane is 1 (8-12).