• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Urea and formaldehyde are mixed in a mole ratio of about 1:2. The mixture is condensed for 30 minutes at a pH of 7.0 to 7.4 and a temperature between 80 DEG and 85 DEG C. The condensation is continued at a pH of 4.8 to 5.8 at the same temperature until the viscosity reaches values between 15 and 50 mPa.s. The mole ratio of urea to formaldehyde is adjusted to a value of 1:1.80 to 1:1.90 by adding urea. The condensation is continued under acidic conditions at the same temperature, until the viscosity reaches values of 35 to 80 mPa.s. At a pH of 5.8 to 6.5, the mole ratio of urea to formaldehyde is adjusted to a value between 1.0:1.0 and 1.0:1.30 by adding urea. The temperature is allowed to drop freely. When the temperature has dropped to below 50 DEG C., the pH is adjusted to a value of 7.0 to 8.0.
    公开号:SU1454254A3
    申请号:SU843823258
    申请日:1984-12-07
    公开日:1989-01-23
    发明作者:Ше Конг Хо
    申请人:Энигма Н.В. (Фирма)；
    IPC主号:
    专利说明:


    cm
    The invention relates to the preparation of urea-formaldehyde resins used for the manufacture of plywood.
    The purpose of the invention is to reduce the free formaldehyde content of urea formaldehyde resin,
    Example 1. Use a reactor with a stirrer, Rea.ktsionnun) the mixture is stirred during: condensation. 2500 kg of 40% formalin and neutral are loaded into the reactor: 40% sodium hydroxide solution is dissolved to pH 7.4 with constant stirring. 1000 kg of urea is added, then the mixture is heated to 82-. At this temperature, the pH is adjusted to 7.2. Condensation is carried out under the same conditions for 30 minutes. After this pH is adjusted to 5.4 with formic acid solution. Condensation is continued at the same temperature until the viscosity of the reaction mixture. will reach 28 mP as measured on a Brookfield viscometer (spindle number 1) at
    Immediately add a second portion of 100 kg of urea. Condensation is carried out at the same temperature until the viscosity of the reaction mixture according to Brookfield (Spivdel No. 1) reaches 68 mP at. Then the pH of the reaction mixture is adjusted to 6.1 by adding 40% sodium hydroxide solution.
    A third urea portion of 640 kg is added so that the final molar ratio of the total formaldehyde to the total urea is 1.15: 1. The heat supply is stopped, and the final stage of condensation is carried out for 25 minutes only with stirring. At the end of this time, the temperature of the reaction mixture drops to about
    The reaction mixture is evaporated under some vacuum at 54-57 ° C to 65.8% of the solid part. It is then cooled to about 38 ° C, and the final pH is adjusted to 7.1 with 40% sodium hydroxide solution. The resulting product is stored at about
    Example 2 A 2500 kg of 40% formalin is loaded into a stirred reactor and first neutralized with a 40% solution of sodium hydroxide to a pH of 7.4 with constant stirring. Then 1000 kg of urine is added.
    five
    0
    five
    0
    five
    0
    five
    0
    five
    and the mixture is heated to 85 ° C. At this temperature, the pH is adjusted to 7, 1, and the reaction mixture is condensed for 30 minutes. After this, the pH is adjusted to 4.8 with a solution of formic acid. Condensation is continued until the viscosity of the reaction mixture according to Brookfield reaches 24 mP (spindle number 1) at 65 ° C,
    After that, a second portion of urea 110 kg is added. Condensation is continued until the viscosity of the reaction mixture according to Brookfield (spindle I 1) reaches about 40 mP at. At this stage, the pH is adjusted to 5.8 with 40% sodium hydroxide solution.
    A third urea portion of 223 kg is added, maintaining the temperature in the reactor. Condensation is continued until the viscosity of the Brookfield blend mixture (Pindeal No. 1) reaches about 50 mP at 65 ° C. The pH is adjusted to 6.2 with 40% sodium hydroxide solution. Heating stops.
    A fourth portion of 46 kg of urea is added so that the final mo. The ratio of total formaldehyde to total urea is not 1.10: 1. The temperature is allowed to drop spontaneously in 20 minutes. The reaction mixture is then cooled to about, and then the pH is adjusted to 7.2 with 40% sodium hydroxide solution. The resulting resin is cooled to 20 ° C and stored at this temperature. The resin is suitable for chipboard production.
    Example 3, is charged to the reactor under stirring conditions of 3600 May, h, formaldehyde at a concentration of 37% and the pH is adjusted to 7.5 with sodium hydroxide. The content is 1332 May, hours. urea with stirring for the whole time and heat the mixture until the temperature is reached. At this temperature the pH is adjusted to 7.0. Under these conditions condensation takes place for 30 minutes. After that, using a solution of formic acid, the pH is adjusted to 5.8. Condensation is continued at the same temperature until the reaction mixture has
    bone 15. MP With measured on a Brookfield viscometer at 65 ° C.
    Immediately add the second portion of 14 mph. urea. The condensation is continued at the same temperature until the reaction mixture has a Brookfil viscosity of about 35 mPa-s, determined at 65 s, the pH of the reaction mixture is then adjusted to 6.5 with the addition of sodium hydroxide solution,
    The third portion of 1184 wt.h. The urea is added in such a way that the final molar ratio of fromaldehyde to the total amount of urea is 1.0: 1.0. The heating is stopped and the final condensation step is carried out for 25 minutes with only one stirring. At the end of this time period, the temperature of the reaction mixture drops to approximately, the reaction mixture is evaporated under partial vacuum at 57-59 s to a residue of 67% solids. It is then cooled to approximately and the final pH is adjusted to 7.0. The product is stored at approximately.
    Example 4. Loaded into the reactor under mixing conditions
    3600 ma.ch. parts of formaldehyde with a concentration of 37% and sodium hydroxide is added to neutralize the solution. 1332 mac by weight is added to the contents. urea with constant stirring and heat the mixture to






    The third portion of 647 ma.ch. the ureas are added in such a way that the final ratio of the total formaldehyde content to the urea content is 1.3: 1. Heating is stopped and the final condensation stage is carried out for 25 minutes with only one
    Zero mixing. At the end of it
    during the period of time, the temperature of the reaction mixture decreases to approximately 57 ° C.
    The reaction mixture is charged under
    5 with partial vacuum at 54-58 ° C until the solids content is 64%. It is then cooled to approximately and the final pH is adjusted to 8.0. The product is stored at
    0 temperature is approximately.
    The data for examples 1-4 are given in table. one.
    Properties urea-formaldehyde 5 resins obtained in examples 1 and 2, are presented in table. 2. The content of free formaldehyde is determined by the sulfite method. For both resins
    it is lower than 0.15%.
    The properties of wood-etry plates produced on the basis of urea-formaldehyde resins of examples 1 and 2 are presented in table. 3
    Properties of urea-formaldehyde resins obtained in examples 4 and 5 are presented in table. 4. The content of free formaldehyde is determined by the sulfite method. For both resins
    achieve 85 C. At this temperature dd lower than 0.15%. The pH is adjusted to 7.4. Under these conditions, condensation is carried out for 30 minutes. After that, the pH was adjusted to 5.0 with formic acid solution. Condensation is continued at 45 at the same temperature until the reaction mixture has a viscosity of 50 mPa-s, determined on a Brookfield viscometer at.
    To the contents immediately add the second amount of 70 wt.h. urea. The condensation is continued at the same temperature until the reaction mixture reaches about 80 mPa s, determined at 65 ° C in Brookfield quality, the pH of the reaction mixture is then adjusted to 5.8 by adding sodium hydroxide solution
    The properties of wood-based on pho rmaldehyde resins are presented in Table.
    权利要求:
    Claims (1)
    [1]
    Formula iso
    The method of obtaining the CQ dehydrogenous resin of conden and formaldehyde in acidity while heating, with a decrease in the content of cedardehyde in the resin, the maldehyde is mixed in a 1: 2 ratio and heated. in an alkaline environment, Dov 7.4 and conducted condensation
     lower than 0.15%.
    The properties of particle boards made on the basis of urea-phosphormaldehyde resins of Examples 3-5 are presented in Table. five.
    Invention Formula
     lower than 0.15%.
    The method of obtaining urea-formaldehyde resin by condensation of urea and formaldehyde in a medium with variable acidity when heated, which differs in that, in order to reduce the content of free formaldehyde in the resin, urea and formaldehyde are mixed in a molar ratio of 1: 2 and heated to 80-85 C in an alkaline medium, the pH is adjusted to 7.0-7.4 and condensation is carried out for
    51454254.
    30 min with subsequent decrease in pH BEFORE | The viscosity is 35-80 mP;
    4.8-5.8 and condensation to a viscosity of 15-50 mP, then add urea
    pH to 5.3-6.5, urea is added to the molar ratio of urea
    to a molar ratio of urea and formaldehyde of 1: 1.0-1.3 followed by formaldehyde 1: 1.8-1.9 and condensation is carried out in an acidic medium until the temperature is lowered to 35 and the pH is adjusted to 7.0 -8.0.
    Molar ratio
    Temperature, with pH
    Condensation time, min
    pH
    Viscosity, mPa with
    Molar ratio U / F
    Viscosity MPN S
    Molar ratio U / F
    pH
    Temperature, ° С pH
    Properties
    Molar ratio
    form dehydrate to
    urinine
    Solid content
    parts%
    Characteristic
    viscosity at
    Brookfield Viscosity
    with (spindle number
    MP
    viscosity 35-80 mb, argument
    pH to 5.3-6.5, urea is added to the molar ratio of urea
    and formaldehyde 1: 1.0–1.3 with a subsequent decrease in temperature to 35– and bringing the pH to 7.0–8.0.
    Table 1
    1: 2
    82-83
    7.2
    thirty
    5.4 28
    .82
    68
    1: 1.15 6.1 38 7.1
    1: 2
    85
    7.1
    30 4.8
    24
    1: 1,8 40
    1: 1.12 5.8 35 7.2
    1; 2
    IN
    7.0
    thirty
    5.8
    15
    1: 1,8
    35
    1: 1 6.5 35 7.0
    1: 2. 85
    7.4
    thirty
    5.0
    50
    1: 1, 9 80
    1: 1.3 5.8 30 8.0
    Table 2 Indicators for example
    r i ZEZTi:
    1.10: 1
    50.2
    1.21
    182
    PH
    Free formaldehyde content, May.%
    Stability at 20 s
    of the week
    Urea formaldehyde resin,%
    Hardener ()
    Gel time
    in depth with
    Surface gelation time at lOOf s
    Bending strength, N / mm
    /
    Internal communication
    N / mm
    I
    Free formaldehyde content, mg HCN / 100 g plate
    1, 0: 1.0 1,
    6764
    1, 31 1.30
    7.1
    7.2
    0.13
    Oh 11
    100 1
    86
    250
    19.7
    0.51
    8.7
    91454254 0
    Continuation of table.4 Properties Indicators for example
    ....... ZIEZEZZI
    Brookfield Viscosity
    with (spindle 9 1), MP 720. 700
    pH7.0. . 8.0
    Content free
    formaldehyde, wt.% 0.11 0.14
    Stability when
    of the week
    Table5 Properties Indicators by Example
    izrjzi :::::
    Urea formaldehyde resin,%
    Hardener ()
    Gel time in depth at, with
    Gel time
    on the surface with
    Bending strength, N / mm Internal communication, N / mm
    Free formaldehyde content, mg HCN / 100 g plate
    Thickness swelling,%, after 2 h
    24 h
    100 1.5
    IN
    410
    20.3
    0.56
    ten
    10 17
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    同族专利:
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    引用文献:
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    RU2537620C2|2013-04-25|2015-01-10|Вячеслав Ефимович Цветков|Method of manufacturing carbamidoformaldehyde oligomer|US2810710A|1955-06-10|1957-10-22|Borden Co|Urea formaldehyde condensation product|
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    DE2334380C2|1973-07-06|1975-04-30|Basf Ag, 6700 Ludwigshafen|
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    IT1209203B|1980-04-10|1989-07-16|Montedison Spa|UREIC NECKLACE WITH LOW DEVELOPMENT OF FORMALDEHYDE AND HIGH TACK VALUE.|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    GB08332962A|GB2150939B|1983-12-09|1983-12-09|A process for preparing urea-formaldehyde resins|
    CN85104298A|CN1005718B|1983-12-09|1985-06-04|Process for preparing vrea-formaldehyde resin having very low mole ratio of formaldehyde to urea|
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