Defoaming agent for sand-containing foam and method for producing the same

Abstract

The application discloses a defoaming agent for sand-containing foam, and a preparation method of the defoaming agent for sand-containing foam, which comprises the following components in percentage by mass: 45-60% of phenylalanine modified silicone oil, 4-5% of white carbon black, 10-20% of low-molecular inorganic flocculant, 2-5% of emulsifier, 3-5% of penetrating agent, 1-3% of viscosity reducer, and the balance of water, wherein the sum of the percentage by mass of the above components is 100%. The phenylalanine modified silicone oil is heated to 90-100 DEG C, and the white carbon black is added while stirring; the mixed solution after stirring is cooled to 70-80 DEG C to obtain intermediate product A. The water is heated to 70-80 DEG C, and the low-molecular inorganic flocculant is added and stirred; the mixed solution after stirring is added with the emulsifier, the penetrating agent and the viscosity reducer to obtain intermediate product B. The intermediate product B is added to the intermediate product A under the reaction conditions of 70-80 DEG C of temperature and 300-500 rpm of rotating speed, and is stirred and cooled to room temperature to obtain the defoaming agent for sand-containing foam, thereby solving the problem of low defoaming efficiency for sand-containing foam.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of defoaming agents, and relates to a defoaming agent for sand-containing foam. BACKGROUND

[0002] During the foam drainage process of a sand-prone gas well, the foam on the ground is often not completely defoamed, leading to the foam turning over in the separator and affecting the downstream production. Taking the Ebegai gas field as an example, the reservoir is characterized by loose cementation, poor diagenesis, interbedded gas and water, strong sensitivity and medium-strong water sensitivity, and is prone to sand production, with sand particle size of 0.04-0.07 mm and clay content of 20%-30%. It is found in the field that the foam formed in the foam drainage well is difficult to eliminate. The defoaming agents in the prior art, such as CN108726913A “Silicone ether composite defoaming agent and preparation method and application thereof”, CN109200632A “Multifunctional non-toxic high-temperature organic silicon modified polyether industrial defoaming agent and preparation method thereof”, and CN109173351A “Emulsion type organic silicon modified castor oil polyether defoaming agent and preparation method thereof”, do not have a special defoaming function for sand-containing foam, and various defoaming agents used in the field do not have obvious effects.

[0003] Therefore, it is necessary to develop a defoaming agent suitable for sand-containing foam to solve the technical problem of poor defoaming effect of the defoaming agent in the prior art on sand-containing foam. SUMMARY

[0004] The application aims to provide a defoaming agent for sand-containing foam, and solve the technical problem of poor defoaming effect of the defoaming agent in the prior art on sand-containing foam.

[0005] Another object of the application is to provide a preparation method of the defoaming agent.

[0006] The technical scheme adopted by the application is to provide a defoaming agent for sand-containing foam, which is composed of the following components in terms of mass percentage: phenylalanine modified silicone oil 45%-60%, white carbon black 4%-5%, low-molecular inorganic flocculant 10%-20%, emulsifier 2%-5%, penetrating agent 3%-5%, viscosity reducer 1%-3%, and the balance being water, and the sum of the mass percentages of the above components is 100%.

[0007] The application is also characterized in that the molecular structure of the phenylalanine modified silicone oil is as shown below, wherein n is 8-16.

[0008]

[0009] The white carbon black is precipitated silicon dioxide with a specific surface area of 150-250 m 2 / g, the low molecular inorganic flocculants are any one of potassium aluminum sulfate, aluminum chloride, ferric sulfate and ferric chloride, the penetrating agent is any one of succinyl sodium sulfonate, edetate sodium sulfate and derivatives thereof, the viscosity reducer is ethylene glycol monobutyl ether, and the emulsifier is any one of non-ionic surfactants with HLB value of 10-14, selected from polyoxyethylene lauryl ether, polyoxyethylene alkyl phenol and polyoxyethylene monolaurate.

[0010] Another technical solution adopted by the present application is to provide a preparation method of the defoaming agent, comprising the following steps:

[0011] Step 1: the following components are weighed respectively according to mass percentage: phenylalanine modified silicone oil 45-60%, white carbon black 4-5%, low molecular inorganic flocculant 10-20%, emulsifier 2-5%, penetrating agent 3-5%, viscosity reducer 1-3%, and the balance is water, the sum of the mass percentages of the above components is 100%;

[0012] Step 2: the phenylalanine modified silicone oil is heated to 90-100℃, and the white carbon black is added while stirring at a speed of 300-500 rpm, and the stirring is performed for 0.5-1 h, and then the mixed solution after stirring is cooled to 70-80℃ to obtain intermediate product A;

[0013] Step 3: the water is heated to 70-80℃, the low molecular inorganic flocculant is added, and stirring is performed at a speed of 300-500 rpm, and the stirring is performed for 15-30 min, and then the emulsifier, the penetrating agent and the viscosity reducer are added to the mixed solution after stirring to obtain intermediate product B;

[0014] Step 4: under the reaction conditions of temperature 70-80℃ and stirring speed 300-500 rpm, the intermediate product B is added to the intermediate product A, and stirring is performed for 1-1.5 h, and then the temperature is lowered to room temperature to obtain the defoaming agent for sand-containing foam.

[0015] The present application has the following advantages:

[0016] (1) the defoaming agent for sand-containing foam prepared by the present application has good storage stability, and does not separate after being placed at 10-40℃ for 6 months;

[0017] (2) the defoaming agent for sand-containing foam prepared by the present application has good dispersion, and can be quickly dispersed in water under manual stirring without obvious separation;

[0018] (3) the defoaming agent for sand-containing foam prepared by the present application has good defoaming effect, and can achieve complete defoaming under the condition that the sand content is 0-2% and the defoaming agent is 0.5-3 times the amount of the foaming agent, the initial defoaming rate is 99%, and the defoaming rate is 100% after 3 min; the technical problem of easy secondary foaming and poor defoaming effect of the defoaming agent for sand-containing foam in the prior art is solved. BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 This is the synthesis reaction equation for the phenylalanine-modified silicone oil of the present invention. Detailed Implementation

[0020] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments.

[0021] The defoamer for sand-containing foam is composed of the following components by mass percentage: 45%–60% phenylalanine-modified silicone oil, 4%–5% silica, 10%–20% low-molecular-weight inorganic flocculant, 2%–5% emulsifier, 3%–5% penetrant, 1%–3% viscosity reducer, and 1%–3% water, with the sum of the mass percentages of all components being 100%. The molecular structure of the phenylalanine-modified silicone oil is shown below, where n ranges from 8 to 16.

[0022]

[0023] like Figure 1 The synthetic equation for phenylalanine-modified silicone oil is shown, which describes the preparation of silicone oil and phenylalanine by reacting them under conditions of sulfoxide and dichloromethane. Among these conditions... It is silicone oil. The components are phenylalanine (SOCl2), thionyl chloride (SOCl2), and dichloromethane (DCM). They spread on the surface of the foam film, acting as defoamers. The low-molecular-weight inorganic flocculant is at least one of potassium aluminum sulfate, aluminum chloride, ferric sulfate, and ferric chloride, which mainly flocculates negatively charged sand into clumps, allowing them to settle by gravity, thus promoting the defoaming of sand-containing foam. The viscosity reducer is ethylene glycol monobutyl ether, which lowers the viscosity of the foam film, thereby increasing the drainage rate on the surface of the foam film and improving the defoaming rate. The emulsifier is a nonionic surfactant with an HLB value of 10-14, selected from at least one of polyoxyethylene lauryl ether, polyoxyethylene alkylphenol, and polyoxyethylene monolaurate, to emulsify the components into a homogeneous phase. The silica is precipitated silica with a specific surface area of ​​150-250 m² / g. 2 / g. Utilizing its silanol bonds to form hydrogen bonds with water molecules, the phenylalanine-modified silicone oil is dispersed and stabilized in water. The further penetrant is at least one of sodium succinate sulfonate, sodium edetate, and their derivatives: its function is to disperse the phenylalanine-modified silicone oil and further improve the defoaming effect.

[0024] The present invention relates to a method for preparing a sand-containing foam defoamer, which is implemented according to the following steps:

[0025] Step 1: Take the following components by mass percentage: phenylalanine modified silicone oil 45%~60%, white carbon black 4%~5%, low molecular inorganic flocculant 10%~20%, emulsifier 2%~5%, penetrant 3%~5%, viscosity reducer 1%~3%, and the balance is water, the sum of the mass percentages of the above components is 100%;

[0026] Step 2: Heat the phenylalanine modified silicone oil to 90~100℃, and add white carbon black while stirring at a speed of 300~500rpm, stir for 0.5~1h, and then cool the mixed solution to 70~80℃ to obtain intermediate product A;

[0027] Step 3: Heat the water to 70~80℃, add the low molecular inorganic flocculant, and stir at a speed of 300~500rpm, stir for 15~30min, then add the emulsifier, penetrant, and viscosity reducer to the mixed solution after stirring to obtain intermediate product B;

[0028] Step 4: Under the reaction conditions of temperature 70~80℃ and stirring speed 300~500rpm, add intermediate product B to intermediate product A, stir for 1~1.5h, and then cool to room temperature to obtain the defoaming agent for sand-containing foam.

[0029] Example 1:

[0030] Preparation of phenylalanine modified silicone oil: 458g of silicone oil with n=10 is reacted with 330g of phenylalanine under the condition of 330g of dichloro sulfoxide and 165g of dichloromethane to prepare, and the synthesis equation is as follows:

[0031]

[0032] The specific implementation is as follows: 458g of silicone oil with n=10, 330g of phenylalanine, and 165g of dichloro sulfoxide are sequentially added to a reaction flask and mixed uniformly to obtain mixture A; 165g of dichloro sulfoxide and 165g of dichloromethane are mixed uniformly in a titration container to obtain mixture B; the stirrer in the reaction flask containing mixture A is turned on, the stirring speed is 200rpm, mixture B is added dropwise to mixture A, the dropping is completed in 30min, and the stirring is continued for 60min; the reaction flask is heated to 60℃ constant temperature, and the reaction solvent is evaporated, and the residue obtained after evaporation for 2h is the prepared phenylalanine modified silicone oil.

[0033] Preparation of defoaming agent for sand-containing foam:

[0034] Step 1: Heat 200g of the above prepared phenylalanine modified silicone oil to 90℃, slowly add 16g of precipitated silica with an average specific surface area of 150m 2 / g under the condition of 400rpm, stir for 1h, and cool to 70℃ to obtain intermediate product A;

[0035] Step 2: 109 g of water was heated to 70°C, 48 g of potassium aluminum sulfate was added under the condition of 400 rpm, stirred for 20 min, then 12 g of polyoxyethylene lauryl ether, 12 g of sodium succinimide and 4 g of ethylene glycol monobutyl ether were added, and stirring was continued for 1 h to obtain intermediate product B;

[0036] Step 3: Intermediate product B was added to intermediate product A under the condition of 70°C and 400 rpm, and stirring was continued for 1 h, and then the temperature was lowered to room temperature to obtain the defoaming agent for sand-containing foam.

[0037] Example 2:

[0038] Preparation of phenylalanine modified silicone oil: 546 g of the above-mentioned silicone oil with n = 12 was reacted with 330 g of phenylalanine in the presence of 330 g of dichloro sulfoxide and 165 g of dichloromethane to prepare, and the synthesis equation is as follows:

[0039]

[0040] The above-mentioned 546 g of silicone oil with n = 12, 330 g of phenylalanine, and 165 g of dichloro sulfoxide were sequentially added to a reaction flask and mixed uniformly to obtain mixture A; 165 g of dichloro sulfoxide and 165 g of dichloromethane were mixed uniformly in a titration container to obtain mixture B; the stirrer in the reaction flask containing mixture 1 was turned on, the stirring speed was 150 rpm, mixture 2 was added dropwise into mixture 1, the dropping was completed in 30 min, and stirring was continued for 50 min; the reaction flask was heated to 60°C and kept at this temperature, and the reaction solvent was evaporated, and after evaporation for 2 h, the remaining substance was the prepared phenylalanine modified silicone oil.

[0041] Preparation of a defoaming agent for sand-containing foam:

[0042] Step 1: 220 g of the prepared phenylalanine modified silicone oil was heated to 95°C, 18 g of precipitated silica with an average specific surface area of 200 m 2 / g was slowly added under the condition of 300 rpm, stirring was continued for 1 h, and then the temperature was lowered to 80°C to obtain intermediate product A;

[0043] Step 2: 82 g of water was heated to 80°C, 40 g of aluminum chloride was added under the condition of 300 rpm, stirring was continued for 15 min, then 16 g of polyoxyethylene alkyl phenol, 16 g of edetate sodium sulfate and 8 g of ethylene glycol monobutyl ether were added, and stirring was continued for 0.5 h to obtain intermediate product B;

[0044] Step 3: Intermediate product B was added to intermediate product A under the condition of 80°C and 300 rpm, and stirring was continued for 1 h, and then the temperature was lowered to room temperature to obtain the defoaming agent for sand-containing foam.

[0045] Example 3:

[0046] Preparation of phenylalanine modified silicone oil: 634g, n is 16 of silicone oil and 330g phenylalanine are reacted under the condition of 330g dichloro sulfoxide and 165g dichloromethane to prepare, the synthesis equation is:

[0047]

[0048] The specific implementation is: 634g, n is 14 of silicone oil, 330g phenylalanine, 165g dichloro sulfoxide are sequentially added into a reaction flask and uniformly mixed to obtain a mixture A; 165g dichloro sulfoxide and 165g dichloromethane are uniformly mixed in a titration container to obtain a mixture B; the stirrer in the reaction flask containing the mixture A is turned on, the stirring speed is 150rpm, the mixture B is added dropwise into the mixture A, the dropwise addition is completed in 30min, and the stirring is continued for 50min; the reaction flask is heated to 60℃ constant temperature, and the reaction solvent is evaporated, and the residue obtained after evaporation for 2h is the prepared phenylalanine modified silicone oil.

[0049] Preparation of defoamer for sand-containing foam:

[0050] Step 1: 212g of the prepared phenylalanine modified silicone oil is heated to 100℃, 20g of precipitated silica with an average specific surface area of 220m 2 / g is slowly added under the condition of 350rpm, stirring for 45min, and cooling to 75℃ to obtain an intermediate product A;

[0051] Step 2: 82g of water is heated to 75℃, 36g of potassium aluminum sulfate and 36g of aluminum chloride are added under the condition of 350rpm, stirring for 20min, and then 8g of polyoxyethylene lauryl ether and 8g of polyoxyethylene alkyl phenol, 8g of succinyl octyl sulfonate, 8g of edetate sodium sulfate and 6g of ethylene glycol monobutyl ether are added, and the stirring is continued for 45min to obtain an intermediate product B;

[0052] Step 3: under the condition of 75℃ and 350rpm, the intermediate product B is added into the intermediate product A, the stirring is continued for 1.5h, and the temperature is cooled to room temperature to obtain the defoamer for sand-containing foam.

[0053] Example 4:

[0054] Preparation of phenylalanine modified silicone oil: 634g, n is 16 of silicone oil and 330g phenylalanine are reacted under the condition of 330g dichloro sulfoxide and 165g dichloromethane to prepare, the synthesis equation is:

[0055]

[0056] The specific implementation is: 370 g of silicon oil with n=8, 330 g of phenylalanine, and 165 g of dichloro sulfoxide are sequentially added into a reaction flask and uniformly mixed to obtain a mixture 1; 165 g of dichloro sulfoxide and 165 g of dichloromethane are uniformly mixed in a titration container to obtain a mixture 2; the stirrer in the reaction flask containing the mixture 1 is turned on, the stirring speed is 100 rpm, the mixture 2 is added dropwise into the mixture 1, the dropwise addition is completed in 30 min, and the stirring is continued for 50 min; the reaction flask is heated to 60 ℃ and kept at this temperature, and the reaction solvent is evaporated, and the residue obtained after evaporation for 2 h is the phenylalanine modified silicon oil.

[0057] Preparation of a defoaming agent for sand-containing foam:

[0058] Step 1: 240 g of the phenylalanine modified silicon oil prepared above is warmed to 90 ℃, 20 g of precipitated silica with an average specific surface area of 250 m 2 / g is slowly added under the condition of 500 rpm, stirring for 0.5 h, and cooling to 70 ℃ to obtain an intermediate product A;

[0059] Step 2: 82 g of water is warmed to 70 ℃, 32 g of potassium aluminum sulfate, 8 g of aluminum chloride, and 4 g of ferric chloride are added under the condition of 500 rpm, stirring for 30 min, and then 6 g of polyoxyethylene lauryl ether, 6 g of polyoxyethylene alkyl phenol, 6 g of polyoxyethylene monolaurate, 8 g of succinylated castor oil sulfonate, 8 g of edetate sodium sulfate, and 4.8 g of ethylene glycol monobutyl ether are added, and the stirring is continued for 1 h to obtain an intermediate product B;

[0060] Step 3: The intermediate product B is added to the intermediate product A under the condition of 70 ℃ and 500 rpm, the stirring is continued for 1.25 h, and the temperature is cooled to room temperature to obtain the defoaming agent for sand-containing foam.

[0061] The defoaming performance of the defoaming agent for sand-containing foam is tested, and the results are as follows:

[0062] At room temperature, 10 g of CaCl2 and 40 g of NaCl are used to prepare 1000 mL of mineralized water, and an effective concentration of 30% of dodecyl dimethyl betaine and mineralized water is used to prepare a 5 g / L aqueous solution, and a certain amount of sand with a particle size of 0.04-0.07 mm is added; 100 mL of the aqueous solution is taken and added to a stirring container, a high-speed stirring method is used to stir at a speed of 11000 r / min for 1 min, and then poured into a 500 mL graduated cylinder, and the initial and static 3 min foam volumes are recorded as V0 and V3, respectively. According to the above method, different amounts of defoaming agent are added to the aqueous solution, and the initial and static 3 min foam volumes are retested as V0def and V3def, respectively.

[0063] The defoaming rate is calculated by the following formula:

[0064] The initial defoaming rate η0is:

[0065] The defoaming rate η3at 3 min is:

[0066] The defoaming experiment results of Examples 1-4 are shown in the following table:

[0067]

[0068]

[0069] It can be seen that, under the condition of sand content of 0-2%, the defoaming agent dosage of 0.5-3 times can achieve complete defoaming, the initial defoaming rate is 99%-99.4%, and the 3 min defoaming rate is 100%.

Claims

1. Defoaming agent for sand-containing foams, characterized in that According to the mass percentage, it is composed of the following components: phenylalanine modified silicone oil 45%~60%, white carbon black 4%~5%, low molecular inorganic flocculants 10%~20%, emulsifier 2%~5%, penetrant 3%~5%, viscosity reducer 1%~3%, the balance is water, the sum of the mass percentage of each component is 100%; The molecular structure of the phenylalanine modified silicone oil is as follows, Wherein n is 8~16.

2. The defoaming agent for sand-containing foam according to claim 1, characterized by, The white carbon black is precipitated silica, and the specific surface area is 150~250m² / g.

3. The defoaming agent for sand-containing foam according to claim 1, characterized by, The low molecular inorganic flocculants are any one of potassium aluminum sulfate, aluminum chloride, ferric sulfate and ferric chloride.

4. The defoaming agent for sand-containing foam according to claim 1, characterized by, The penetrant is any one of succinyl sodium, edetate sodium sulfate and its derivatives.

5. The defoaming agent for sand-containing foam according to claim 1, characterized by, The viscosity reducer is ethylene glycol monobutyl ether.

6. The defoaming agent for sand-containing foam according to claim 1, characterized by, The emulsifier is a non-ionic surfactant with an HLB value of 10~14, and any one of polyoxyethylene lauryl ether, polyoxyethylene alkyl phenol and polyoxyethylene monolaurate is selected.

7. A process for the preparation of an antifoam for sand-containing foams, characterized in that The above defoaming agent It comprises the following steps: step 1: according to the mass percentage, the following components are weighed respectively: phenylalanine modified silicone oil 45%~60%, white carbon black 4%~5%, low molecular inorganic flocculants 10%~20%, emulsifier 2%~5%, penetrant 3%~5%, viscosity reducer 1%~3%, the balance is water, the sum of the mass percentage of each component is 100%; Step 2: the phenylalanine modified silicone oil is heated to 90~100℃, and the white carbon black is added while stirring, and the mixed liquid after stirring is cooled to 70~80℃, to obtain intermediate product A; Step 3: the water is heated to 70~80℃, the low molecular inorganic flocculants are added, and the mixed liquid after stirring is added with emulsifier, penetrant and viscosity reducer to obtain intermediate product B; Step 4: under the reaction conditions of temperature 70~80℃ and rotation speed 300~500rpm, intermediate product B is added to intermediate product A, and stirred to room temperature to obtain the defoaming agent for sand-containing foam.

8. The method for preparing a defoamer for sand-containing foams according to claim 7, characterized in that, The stirring rate of step 2 is 300~500rpm, and the stirring time is 0.5~1h.

9. The method for preparing a defoamer for sand-containing foams according to claim 7, characterized in that, The stirring rate of step 3 is 300~500rpm, and the stirring time is 15~30min.

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